CN113213969A - Pretreatment method of crucible for smelting sintered neodymium iron boron and preparation method of sintered neodymium iron boron - Google Patents
Pretreatment method of crucible for smelting sintered neodymium iron boron and preparation method of sintered neodymium iron boron Download PDFInfo
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- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details peculiar to crucible or pot furnaces
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- 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
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- 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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- 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
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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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Abstract
The invention relates to the technical field of sintered neodymium iron boron smelting, and discloses a pretreatment method of a crucible for sintered neodymium iron boron smelting and a preparation method of sintered neodymium iron boron, aiming at the problems that the crucible is etched and pits or cracks are generated due to the fact that Al and the like are easily introduced in the existing crucible repairing method; uniformly mixing the filling material and the mineral binder to prepare a coating material; uniformly coating the coating material on the inner surface of the crucible to form a coating film layer; heating the crucible and the coating film layer to dry the coating film layer; the filling material is at least one of zirconium oxide, niobium oxide and titanium oxide powder. The pretreatment method of the crucible can effectively avoid the introduction of Al and the like, and improve the service life of the crucible and the efficiency of cleaning the crucible. Meanwhile, the performance fluctuation of the neodymium iron boron magnet which is subjected to paper burning by the method is reduced, and the performance stability is improved.
Description
Technical Field
The invention relates to the technical field of sintered neodymium iron boron smelting, in particular to a pretreatment method of a crucible for sintered neodymium iron boron smelting and a preparation method of sintered neodymium iron boron.
Background
Sintered neodymium iron boron is usually smelted by adopting a crucible fired by mullite, alumina and the like. Since the rare earth in the sintered neodymium iron boron is easy to oxidize and the reaction of rare earth metal and aluminum oxide is easy to generate rare earth oxide and Al, the crucible is etched. The rare earth oxide and the residual molten metal after smelting and casting can be bonded or solidified on the crucible to form slag. Before smelting at every time, slag removal treatment needs to be carried out on the crucible, so that pits or cracks appear on the surface of the crucible, the more the crucible is used, the stronger the binding force between slag and the crucible is, the more difficult the slag is to be removed, and the production efficiency and the safety of the crucible are influenced. In addition, compared with the formula, the components of the melted neodymium iron boron are uncontrollably increased by 0.01-0.2 wt.% of Al, the Al can enter the main phase and the grain boundary phase of the neodymium iron boron, and the coercive force (Hcj) can be increased, but the remanence is obviously reduced, so that the product performance is accidentally fluctuated. Therefore, it is important to pretreat or repair the crucible before each melting.
Chinese patent application CN109974456A proposes a method of repairing a crucible using magnesia as the main repairing agent. However, impurity elements such as magnesium and aluminum are still introduced by using the magnesia, so that the magnet performance of the sintered neodymium-iron-boron magnet in adjacent batches fluctuates.
Disclosure of Invention
Aiming at the problems that Al and the like are easily introduced in the existing crucible repairing method to cause the crucible to be etched and a pit or a crack is generated, the invention aims to provide a pretreatment method of the crucible for smelting sintered neodymium iron boron, which can effectively avoid the introduction of Al and the like, prolong the service life of the crucible and improve the efficiency of cleaning the crucible.
The invention also aims to provide a preparation method of the sintered neodymium iron boron magnet, which is characterized in that the treated crucible is used for preparing the sintered neodymium iron boron magnet, so that the fluctuation of the performance of the magnet is avoided being aggravated, the fluctuation of the performance of the magnet is reduced, and the stability of the magnet is improved.
The invention provides the following technical scheme:
a pretreatment method of a crucible for smelting sintered neodymium iron boron comprises the following steps:
(1) cleaning the surface of the crucible for slagging, and blowing the surface of the crucible clean;
(2) uniformly mixing the filling material and the mineral binder to prepare a coating material;
(3) uniformly coating the coating material on the inner surface of the crucible to form a coating film layer;
(4) heating the crucible and the coating film layer to dry the coating film layer;
wherein the filling material is at least one of zirconium oxide powder, niobium oxide powder and titanium oxide powder.
In the pretreatment method, chromium oxide, niobium oxide or titanium oxide is adopted to pretreat the surface of the crucible, so that the introduction of elements such as Al and the like is avoided. Rare earth oxide and melt are preferentially solidified on the coating layer, so that the binding force of final slag and the crucible is greatly reduced, the difficulty in cleaning the slag is reduced, the operation efficiency is improved, and the service life of the crucible is prolonged.
Preferably, the filler is at least one of titanium oxide and niobium oxide. Through research, the sintered neodymium-iron-boron magnet repaired by using titanium oxide and niobium oxide has smaller performance fluctuation.
Preferably, in the method of the invention, the filling material is a mixture of titanium oxide and niobium oxide, and the mass ratio of the titanium oxide to the niobium oxide is 1: 0.02-0.08. Within the range, the composition of the two materials has the obvious effect of reducing the volatility of the magnetic property of the sintered neodymium iron boron.
Preferably, the mineral binder is a water glass solution.
Preferably, the mineral binder is present in the coating material in a proportion of 0.05 to 5 wt%. When the mass fraction of the water glass is less than 0.05wt%, the coating material is too dry to adhere to the inner wall of the crucible. When the weight ratio of the water glass is more than 5wt%, the coating material has too strong fluidity and flows down along the crucible arm under the action of gravity, and uniform coating cannot be realized.
Preferably, the heating temperature is 700 ℃ or higher. Heating until the coating layer is hot red.
Preferably, the process of the invention is carried out by electric induction heating in a crucible using a pure iron or graphite rod.
Preferably, the method of the present invention further comprises filling cracks and pits in the crucible with a mixture of magnesite and mineral binder in step (1). The coating film layer is arranged below the coating film layer, so that the effect of the coating layer is not influenced, and the coating film is more easily obtained compared with a coating material.
A preparation method of a sintered neodymium-iron-boron magnet comprises the steps of mixing raw materials of the sintered neodymium-iron-boron magnet according to a certain amount, putting the mixture into a crucible treated by the pretreatment method, then putting the crucible into a high-frequency vacuum induction smelting furnace for smelting, and then adopting conventional casting, hydrogen crushing, fine grinding, molding and sintering. The oxides of Zr, Nb and Ti are coated on the surface layer of the crucible, rare earth metal reacts with the oxides during smelting, trace Zr, Nb or Ti is introduced into molten metal, the microstructure can be refined, the grain growth can be inhibited, and the elements do not enter a main phase, so that the stability of the product performance is improved.
The invention has the following beneficial effects:
the pretreatment method of the crucible can effectively avoid the introduction of Al and the like, and improve the service life of the crucible and the efficiency of cleaning the crucible. Meanwhile, the performance fluctuation of the neodymium iron boron magnet which is subjected to paper burning by the method is reduced, and the performance stability is improved.
Detailed Description
The following further describes the embodiments of the present invention.
The starting materials used in the present invention are commercially available or commonly used in the art, unless otherwise specified, and the methods in the following examples are conventional in the art, unless otherwise specified.
The following table 1 shows a description of the preparation of the sintered ndfeb magnet from the raw materials for the sintered ndfeb magnet.
Example 1
A pretreatment method of a crucible for smelting sintered neodymium iron boron comprises the following steps:
(1) cleaning the surface of the crucible for slagging, and blowing the surface of the crucible clean;
(2) uniformly mixing the filling material zirconia powder and a water glass solution to prepare a coating material, wherein the water glass solution accounts for 0.05 wt%;
(3) uniformly coating the coating material on the inner surface of the crucible to form a coating film layer;
(4) and (3) electrically inducing, heating and baking the graphite rod in the crucible, keeping the heating temperature at 700 ℃ and baking for 3h to dry the coating film layer, and finishing the pretreatment of the crucible.
Example 2
The difference between the pretreatment method for the crucible for smelting sintered neodymium iron boron and the embodiment 1 is that the filling material in the step (2) is titanium oxide powder.
Example 3
The difference between the pretreatment method for the crucible for smelting sintered neodymium iron boron and the embodiment 1 is that the filling material in the step (2) is niobium oxide powder.
Example 4
A preparation method of sintered neodymium iron boron comprises the following steps:
(1) weighing the raw materials of the sintered neodymium-iron-boron magnet according to the amount in the following table 1, mixing, putting into the crucible pretreated in the embodiment 1, and refining at 1500 ℃ for 5min in a high-frequency vacuum induction melting furnace;
(2) adjusting heating power to realize cooling until the temperature of the molten liquid reaches the target temperature of 1420 ℃, and casting by using a single-roll quenching method to obtain a melt-spun piece;
(3) putting the melt-spun sheet into a hydrogen breaking furnace at room temperature, introducing hydrogen with the purity of 99.5% into the furnace, absorbing the hydrogen for 2 hours, vacuumizing while heating, vacuumizing at the temperature of 500 ℃ for 2 hours, cooling, and taking out the powder after hydrogen breaking and crushing;
(4) performing jet milling on the powder obtained in the step (3) under nitrogen with the oxygen content of less than 100ppm to obtain fine powder, adding 0.10 wt% of methyl octanoate into the fine powder, and then fully mixing by using a V-shaped mixer;
(5) after being formed in a press with an oriented magnetic field of 1.8T, the material is placed into a sintering furnace for sintering and aging.
Example 5
The difference between the preparation method of the sintered neodymium iron boron and the embodiment 4 is that the crucible used in the step (1) is the crucible pretreated in the embodiment 2.
Example 6
The difference between the preparation method of the sintered neodymium iron boron and the embodiment 4 is that the crucible used in the step (1) is the crucible pretreated in the embodiment 3.
The raw materials of the sintered nd-fe-b magnets prepared in the above examples 4 to 6 are shown in table 1 below.
TABLE 1 raw materials of sintered NdFeB magnets prepared in examples 4 to 6
The performance of the sintered nd-fe-b magnets prepared in examples 4, 5, and 6 was measured by ICP-OES for the composition of the sintered bodies, magnetic performance was measured using the NIM-62000 rare earth permanent magnet nondestructive measurement system of the china measurement institute, each crucible was coated with a dressing and continuously produced for 5 furnaces, and the final performance was averaged, and the results are shown in table 2.
Table 2 detection of composition and magnetic Properties of sintered NdFeB magnets prepared in examples 4-6
Wherein comparative example 1 is a sintered nd-fe-b magnet prepared according to the method of example 4 after pretreating the crucible according to the method of example 1 after preparing the coating material using magnesite and a 0.05wt% water glass solution.
As can be seen from table 2 above, trace amounts of Zr, Ti, or Nb are correspondingly introduced into the sintered nd-fe-b magnet prepared by the method of the present application, and magnetic properties such as Br, Hcj, etc. are not significantly improved as compared with comparative example 1, but the corresponding standard deviation is significantly reduced, which indicates that the prepared sintered nd-fe-b magnet has no performance fluctuation of a corresponding degree, the fluctuation range is greatly reduced, and the performance stability is significantly improved as compared with comparative example 1. Meanwhile, in terms of stability improvement, the use effect of the titanium oxide is optimal among the three.
Example 7
The difference between the pretreatment method for the crucible for smelting sintered neodymium iron boron and the embodiment 1 is that the mass ratio of the water glass solution in the step (2) is 5 wt%.
Example 8
The difference between the pretreatment method for the crucible for smelting sintered neodymium iron boron and the embodiment 2 is that the mass ratio of the water glass solution in the step (2) is 5 wt%.
Example 9
The difference between the pretreatment method for the crucible for smelting sintered neodymium iron boron and the embodiment 3 is that the mass ratio of the water glass solution in the step (2) is 5 wt%.
Example 10
A preparation method of sintered neodymium iron boron comprises the following steps:
(1) weighing the raw materials of the sintered neodymium-iron-boron magnet according to the amount in the following table 1, mixing, putting into the crucible pretreated in the embodiment 1, and refining at 1500 ℃ for 5min in a high-frequency vacuum induction melting furnace;
(2) adjusting heating power to realize cooling until the temperature of the molten liquid reaches the target temperature of 1400 ℃, and casting by using a single-roll quenching method to obtain a melt-spun piece;
(3) putting the melt-spun sheet into a hydrogen breaking furnace at room temperature, introducing hydrogen with the purity of 99.5% into the furnace, absorbing the hydrogen for 2 hours, vacuumizing while heating, vacuumizing at the temperature of 500 ℃ for 2 hours, cooling, and taking out the powder after hydrogen breaking and crushing;
(4) performing jet milling on the powder obtained in the step (3) under nitrogen with the oxygen content of less than 100ppm to obtain fine powder, adding 0.10 wt% of methyl octanoate into the fine powder, and then fully mixing by using a V-shaped mixer;
(5) after being formed in a press with an oriented magnetic field of 1.8T, the material is placed into a sintering furnace for sintering and aging.
Example 11
A method for preparing sintered nd-fe-b, which is different from example 10 in that the pretreated crucible of example 8 is used in step (1).
Example 12
A method for preparing sintered nd-fe-b, which is different from example 11 in that the pretreated crucible of example 9 is used in step (1).
The raw materials of the sintered nd-fe-b magnets prepared in the above examples 10 to 12 are shown in table 3 below.
TABLE 3 raw materials for sintered NdFeB magnets prepared in examples 10 to 12
The properties of the sintered nd-fe-b magnets prepared in examples 10, 11, and 12 were measured by ICP-OES for the composition of the sintered bodies, magnetic properties were measured using the NIM-62000 rare earth permanent magnet nondestructive measurement system of the china measurement institute, each crucible was coated with a dressing and continuously produced for 5 furnaces, and the final properties were averaged, and the results are shown in table 4.
Wherein comparative example 2 is a sintered nd-fe-b magnet prepared according to the method of example 10 after pretreating the crucible according to the method of example 7 after preparing the coating material using magnesite and a 5wt% water glass solution.
As can be seen from table 4 below, even if the raw material components of the sintered ndfeb magnet are changed, the sintered ndfeb magnet prepared by the method of the present application has no performance fluctuation of a corresponding degree, the fluctuation range is greatly reduced, and the performance stability is significantly improved, compared with comparative example 2. Meanwhile, in terms of stability improvement, the use effect of the titanium oxide is optimal among the three.
Table 4 detection of composition and magnetic Properties of sintered NdFeB magnets prepared in examples 10 to 12
Example 13
A method for preparing sintered nd-fe-b, which is different from example 5 in that the crucible used in step (1) is pretreated according to the method of example 2, wherein the filling material is a mixture of titanium oxide and niobium oxide at a mass ratio of 1: 0.01.
Example 14
A method for preparing sintered nd-fe-b, which is different from example 5 in that the crucible used in step (1) is pretreated according to the method of example 2, wherein the filling material is a mixture of titanium oxide and niobium oxide at a mass ratio of 1: 0.02.
Example 15
A method for preparing sintered nd-fe-b, which is different from example 5 in that the crucible used in step (1) is pretreated according to the method of example 2, wherein the filling material is a mixture of titanium oxide and niobium oxide at a mass ratio of 1: 0.06.
Example 16
A method for preparing sintered nd-fe-b, which is different from example 5 in that the crucible used in step (1) is pretreated according to the method of example 2, wherein the filling material is a mixture of titanium oxide and niobium oxide at a mass ratio of 1: 0.08.
Example 17
A method for preparing sintered nd-fe-b, which is different from example 5 in that the crucible used in step (1) is pretreated according to the method of example 2, wherein the filling material is a mixture of titanium oxide and niobium oxide at a mass ratio of 1: 0.1.
Example 18
A method for preparing sintered nd-fe-b, which is different from example 5 in that the crucible used in step (1) is pretreated according to the method of example 2, wherein the filling material is a mixture of titanium oxide and niobium oxide at a mass ratio of 1: 0.5.
Example 19
A method for preparing sintered nd-fe-b, which is different from example 5 in that the crucible used in step (1) is pretreated according to the method of example 2, wherein the filling material is a mixture of titanium oxide and niobium oxide at a mass ratio of 1: 1.
Example 20
A method for preparing sintered nd-fe-b, which is different from example 5 in that the crucible used in step (1) is pretreated according to the method of example 2, wherein the filling material is a mixture of titanium oxide and niobium oxide at a mass ratio of 1: 2.
The results of examining the magnetic properties of the ndfeb magnets prepared in examples 13 to 20 are shown in table 5.
TABLE 5 results of magnetic property measurements of examples 13 to 20
As can be seen from Table 5 above, the use of the compounded titanium oxide and niobium oxide can also achieve the effects of reducing performance fluctuation and improving performance stability, and is generally between the use of titanium oxide and niobium oxide alone. However, when the compounding ratio of titanium oxide and niobium oxide is in the range of 1:0.02 to 0.08, the stability of Hcj can be further improved as shown in examples 14 to 16.
Claims (9)
1. The pretreatment method of the crucible for smelting the sintered neodymium iron boron is characterized by comprising the following steps of:
(1) cleaning the surface of the crucible for slagging, and blowing the surface of the crucible clean;
(2) uniformly mixing the filling material and the mineral binder to prepare a coating material;
(3) uniformly coating the coating material on the inner surface of the crucible to form a coating film layer;
(4) heating the crucible and the coating film layer to dry the coating film layer;
wherein the filling material is at least one of zirconium oxide powder, niobium oxide powder and titanium oxide powder.
2. The pretreatment method of the crucible for sintered nd-fe-b magnet according to claim 1, wherein the filler is at least one of titanium oxide and niobium oxide.
3. The pretreatment method of the crucible for the sintered neodymium-iron-boron magnet according to claim 1, wherein the filling material is a mixture of titanium oxide and niobium oxide, and the mass ratio of the titanium oxide to the niobium oxide is 1: 0.02-0.08.
4. The pretreatment method of a crucible for sintered nd-fe-b magnet according to claim 1, wherein the mineral binder is a water glass solution.
5. The pretreatment method of a crucible for sintered neodymium-iron-boron magnet according to claim 1 or 4, wherein the mass ratio of the mineral binder in the coating material is 0.05wt% to 5 wt%.
6. The pretreatment method of the crucible for sintering neodymium iron boron magnet according to claim 1, wherein the heating temperature is not less than 700 ℃.
7. The pretreatment method of the crucible for sintered nd-fe-b magnet according to claim 1 or 6, characterized in that pure iron rod or graphite rod is used for electric induction heating in the crucible.
8. The pretreatment method of a crucible for sintered nd-fe-b magnet according to claim 1, further comprising filling cracks and pits of the crucible with a mixture of magnesite and mineral binder in step (1).
9. A preparation method of a sintered neodymium-iron-boron magnet is characterized in that raw materials of the sintered neodymium-iron-boron magnet are taken according to the amount, mixed and then placed into a crucible treated by the pretreatment method of any one of claims 1 to 7, then placed into a high-frequency vacuum induction smelting furnace for smelting, and then conventional casting, hydrogen crushing, fine grinding, molding and sintering are adopted.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110419869.XA CN113213969B (en) | 2021-04-19 | 2021-04-19 | Pretreatment method of crucible for smelting sintered neodymium iron boron and preparation method of sintered neodymium iron boron |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110419869.XA CN113213969B (en) | 2021-04-19 | 2021-04-19 | Pretreatment method of crucible for smelting sintered neodymium iron boron and preparation method of sintered neodymium iron boron |
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| Publication Number | Publication Date |
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| CN113213969A true CN113213969A (en) | 2021-08-06 |
| CN113213969B CN113213969B (en) | 2022-06-28 |
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