CN108962525B - Preparation method of magnetic gradient nanostructure on surface layer of sintered neodymium-iron-boron magnet - Google Patents
Preparation method of magnetic gradient nanostructure on surface layer of sintered neodymium-iron-boron magnet Download PDFInfo
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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
- 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
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- 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
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- 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
- H01F41/026—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 protecting methods against environmental influences, e.g. oxygen, by surface treatment
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Abstract
The invention relates to the technical field of surface engineering and laser processing, in particular to a preparation method of a magnetic gradient nano structure on the surface layer of a sintered neodymium-iron-boron magnet. The method comprises the steps of firstly soaking a sintered neodymium-iron-boron magnet in a chlorine-containing solution for a period of time, expanding a grain boundary gap after a grain boundary on the surface layer of the sintered neodymium-iron-boron magnet is corroded, cleaning the surface of the sintered neodymium-iron-boron magnet after corrosion treatment, and then implanting magnetic rare earth metal nano powder into the expanded grain boundary after corrosion through the force effect of laser shock waves by adopting a laser shock strengthening technology, so that a magnetic gradient nano structure is obtained on the surface layer of the sintered neodymium-iron-boron magnet.
Description
Technical Field
The invention relates to the technical field of surface engineering and laser processing, in particular to a preparation method of a magnetic gradient nano structure on the surface layer of a sintered neodymium-iron-boron magnet.
Background
The neodymium iron boron magnet is a magnet king due to excellent magnetic performance, and has the advantages of high magnetic energy and coercive force, high energy density, high cost performance and the like as a rare earth permanent magnet material. However, the ndfeb magnet has many disadvantages, such as low working temperature, poor temperature characteristics, easy pulverization and corrosion, and must be improved by adjusting its chemical composition and adopting a surface treatment method to meet the requirements of practical application. According to the existing research, an effective method for improving the coercive force and high-temperature practicability of the neodymium iron boron magnet is to add a small amount of heavy rare earth metal (such as Dy, Tb and the like) or optimize the process to refine the crystal grains of the magnet. However, the conventional grain boundary diffusion technology is insufficient in terms of cost, processing, and the like. The existing crystal boundary mainly has three main types:
the first type is to coat the surface of a matrix with powder and slurry containing rare earth metal, realize the diffusion of heavy rare earth metal elements along grain boundaries through physical contact diffusion, and improve the coercivity, thereby improving the temperature resistance. The method has the disadvantages that the coating can be adhered to a matrix, so that grinding is needed to be added, the improvement effect on the coercive force is inevitably reduced, and meanwhile, the existing test shows that the diffusion depth is generally within 500 mu m, the grinding accurate grinding can cause the loss of more than 100 mu m of at least two surfaces, and the processing can cause the temperature resistance to be greatly reduced; moreover, due to uneven surface, the problem of processing inclination can be caused, and the magnetic declination is enlarged; because the surface is coated with the coating layer, only a small part of diffusion is actually carried out, so that the waste of a diffusion material is caused, and the production cost is high; the permanent magnet material liquid phase is volatilized when the temperature is higher than 650 ℃ for a long time, and finally the material is inevitably subjected to local liquid phase loss, so that holes and main phase grains are directly connected into a whole, the demagnetization coupling effect of the material is lost, the coercive force is locally influenced to be improved, and the material is easy to lose magnetism locally due to more loss.
The second type is that a very thin rare earth metal layer (generally about 30 μm) is formed on the surface of a substrate by a physical or chemical method by adopting a method such as evaporation plating or magnetron sputtering, but the diffusion source only has a very thin surface, so that the high-concentration diffusion source cannot be continuously provided, and the diffusion effect is influenced; and because long-time high-temperature diffusion is adopted, liquid phase volatilization is caused, the improvement of local coercive force is influenced, and local demagnetization is easy to occur under the condition of deletion.
The third one is that the heavy rare earth metal is not contacted with the base material, the rare earth metal forms gas state under certain temperature (generally 800-1100 ℃) and certain low vacuum degree, continuously diffuses to the surface of the base body, deposits and diffuses, and the diffusion time is longer, and the defects are that: the diffusion is generally carried out at a higher temperature for a long time, and the liquid phase of the neodymium iron boron base material is generated at a temperature of more than 650 ℃, so that the improvement of the coercive force is influenced.
Laser Shock Peening (LSP) is a new type of surface strengthening technique, mainly using short pulses(tens of nanoseconds), high peak power density: (>109W/cm2) The laser beam is irradiated on the metal surface, the laser beam is absorbed by the absorption layer after passing through the constraint layer, the absorption layer obtains energy to form explosive gasification evaporation, high-temperature and high-pressure plasma is generated, and the plasma forms high-pressure shock waves to be transmitted to the interior of the material due to the constraint of the outer constraint layer. The rare earth metal nano powder is clamped between the absorption layer and the base material sintered neodymium iron boron magnet, and under the action of the high-strength shock wave, the rare earth metal nano powder is implanted into the surface layer of the sintered neodymium iron boron magnet to form a magnetic gradient nano structure. In addition, the laser shock nanoparticle implantation only utilizes the force effect of shock waves without thermal effect, so that the improvement of the coercive force of the sintered neodymium iron boron substrate is not influenced, and the sintered neodymium iron boron substrate is not demagnetized. However, the surface of the sintered nd-fe-b magnet has few effective grain boundaries (grain boundary gaps are larger than or equal to the grain size of the rare-earth metal nano powder) in which the rare-earth metal nano powder is implanted, so that the implantation efficiency is not high.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a sintered neodymium iron boron magnet surface layer magnetic gradient nano structure to solve the problems. The method comprises the steps of immersing a sintered neodymium-iron-boron magnet in a chlorine-containing solution for a period of time, expanding a grain boundary gap after a grain boundary on the surface layer of the sintered neodymium-iron-boron magnet is corroded, cleaning the surface of the sintered neodymium-iron-boron magnet after corrosion treatment, and then implanting magnetic rare earth metal nano powder into the expanded grain boundary after corrosion through the force effect of laser shock waves by adopting a laser shock strengthening technology, so that a magnetic gradient nano structure is obtained on the surface layer of the sintered neodymium-iron-boron magnet.
The magnetic rare earth metal nano powder is Dy nano powder or Tb nano powder.
The corrosion treatment process of the chlorine-containing solution comprises the following steps: preparing a NaCl solution with the solute mass fraction of 5-20% at normal temperature, and immersing the sintered neodymium-iron-boron magnet into the prepared chlorine-containing solution for a period of time, wherein the corrosion time is 30-60 min.
The cleaning process after the chlorine-containing solution corrosion treatment comprises the following steps: the surface of the sintered neodymium-iron-boron magnet is washed by deionized water, and then the sintered neodymium-iron-boron magnet is ultrasonically cleaned by the deionized water, so that chlorine-containing solution and corrosion products in a crystal boundary are removed.
The laser shock implantation treatment process comprises the following steps: and adhering a composite absorption layer consisting of a laser absorption layer and a magnetic rare earth metal nano powder layer to a to-be-impacted area on the surface of the sintered neodymium-iron-boron magnet, wherein the composite absorption layer absorbs laser energy to generate plasma shock waves, and under the action of high-pressure impact force, the unvaporized magnetic rare earth metal nano powder particles are implanted into the surface layer of the sintered neodymium-iron-boron magnet.
The composite absorption layer is composed of two parts: the first layer is a laser absorption layer with the thickness of 0.1mm and is used for absorbing laser energy, and the used laser absorption layer is a special aluminum foil for laser shock strengthening produced by American 3M company; the second layer is a nanometer powder layer with the thickness of 0.1-0.2 mm, and is used for providing nanometer powder mask particles implanted into the surface layer of the sintered neodymium-iron-boron magnet, and the components of the nanometer powder mask particles are calculated according to mass fractions: 80 wt% of magnetic rare earth metal nanopowder, 15 wt% of high temperature sealing glue and 5 wt% of an additive for improving the flexibility of the layer of nanopowder particles. The second layer is coated on the first layer.
The additive for improving the flexibility of the magnetic rare earth metal nano powder particle layer such as Dy, Tb and the like comprises the following components: the method comprises the following steps of mixing thinner, glyceride, phthalic anhydride and sebacic acid in a mass ratio of 2: 2: 1: 1, uniformly mixing to prepare the flexible polyester material.
The preparation process of the composite absorption layer comprises the following steps: uniformly mixing magnetic rare earth metal nano powder, high-temperature sealant and an additive in proportion, coating the mixture on a laser absorption layer, placing the composite absorption layer consisting of the laser absorption layer and a nano powder layer in a vacuum environment to remove bubbles, then placing the composite absorption layer in a mold, heating to 70-90 ℃, taking out the composite absorption layer from the mold after cooling, and carrying out vacuum plastic package for later use.
In the laser shock implantation treatment process, the laser process parameters are as follows: the pulse width is 8-30 ns, the pulse energy is 2-10J, the frequency is 1Hz, the diameter of a light spot is 2-3 mm, the number of impact layers is 1-3, a restraint layer is a water film with the thickness of 1-2 mm formed by deionized water flow, and the pulse isHas a peak pressure of P1Pressure at the edge of the light spot is P2Satisfies 2 sigmaH≤P1≤2.5σH，P2≥σHWherein
In the formula (I), the compound is shown in the specification,
and v is the Poisson's ratio of the material, so that the whole laser impact light spot area generates dynamic plastic deformation, and the metal workpiece in the light spot central area does not generate macroscopic deformation.
After the laser shock implantation treatment, under the force effect of laser shock waves, the effective grain boundary that magnetic rare earth metal nano powder expands after corroding through sintered neodymium iron boron magnet surface layer is implanted inside the sintered neodymium iron boron magnet, because the shock waves degressive along the sintered neodymium iron boron magnet depth direction, so, the implantation amount of rare earth metal nano powder also degressive along the depth direction, and the sintered neodymium iron boron magnet surface layer forms magnetic gradient nano structure.
According to the determination of a scanning electron microscope, the gradient nanostructure layer prepared on the surface layer of the sintered neodymium-iron-boron magnet by adopting the preparation method of the magnetic gradient nanostructure on the surface layer of the sintered neodymium-iron-boron magnet has the thickness of 500-1000 microns of the magnetic gradient nanostructure layer on the surface layer and the thickness of a grain refining layer of 500-800 microns.
The invention has the beneficial effects that:
(1) the invention effectively realizes the controllable preparation of the surface magnetic gradient nano structure of the sintered neodymium iron boron magnet and the improvement of the coercive force, and provides a novel and effective method for the implantation of the rare earth metal nano powder in the sintered neodymium iron boron magnet, which is used in the fields of permanent magnet motors, magnetic suspension and the like, in particular the fields of rail transit, wind power generation, new energy automobiles and the like which concern national economy and national defense industry;
(2) the invention can obtain the ideal layer thickness of the sintered neodymium iron boron magnet surface layer magnetic gradient nano structure, and innovatively provides a feasible method by combining the feasibility of the current technology aiming at the limitation of the current technology;
(3) the invention effectively improves the implantation efficiency of the rare earth metal nano powder, improves the utilization rate of the rare earth metal nano powder, and can recycle the non-implanted powder, thereby effectively reducing the cost;
(4) the invention obviously refines the surface crystal grains of the sintered neodymium-iron-boron magnet, further improves the coercive force and the magnetic performance of the sintered neodymium-iron-boron magnet, and can effectively reduce the usage amount of rare earth metals.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the examples or the description of the prior art will be briefly described below.
Fig. 1 is a flowchart of the operation steps of the method for preparing the surface magnetic gradient nanostructure of the sintered nd-fe-b magnet described herein.
FIG. 2 is a schematic drawing of sample dimensions for embodiments herein.
FIG. 3 is a scanning electron micrograph of a cross-section of an embodiment herein.
Fig. 4 is a schematic view of the grain distribution of the cross section of sample 2 cut along the thickness direction line.
FIG. 5 is a graph of the distribution of the coercivity across the cross section of sample 2 along the depth of the sample.
Detailed Description
The following detailed description of the present invention will be made with reference to the accompanying drawings and examples, but the present invention should not be limited to the examples.
An example of the sintered nd-fe-b magnet surface magnetic gradient nanostructure prepared by the above method comprises the following steps:
(1) the sintered nd-fe-b magnet blank is cut into impact test pieces with the size of 20mm × 20mm × 3mm by using wire cutting, two identical test pieces are prepared for comparative test and are respectively marked as test piece 1 and test piece 2, the test piece 1 is not processed, the test piece 2 is an implantation test piece, wherein a square area with the size of 15mm × 15mm is a laser impact processing area, namely an area a, as shown in fig. 2.
(2) And (3) immersing the sample 2 into a prepared NaCl solution with the concentration of 10% at normal temperature, and standing and corroding for 60 min.
(3) And taking out the corroded sample 2 from the chlorine-containing solution, washing the surface of the sample 2 by using deionized water, and ultrasonically cleaning the sample by using absolute ethyl alcohol to remove the chlorine-containing solution and corrosion products in the crystal boundary.
(4) Adhering a composite absorption layer consisting of a laser absorption layer and a Dy magnetic rare earth metal nano powder layer on a region A to be impacted of the sample 2, and carrying out laser shock strengthening treatment on the composite absorption layer, wherein the laser shock strengthening parameters are as follows: the spot shape is circular, the diameter is 3mm, the pulse width is 10ns, the pulse energy is 8J, the transverse and longitudinal lapping rate is 50%, and the number of impact layers is 1. The restraint layer is a water film with the thickness of 1-2 mm formed by deionized water flow, and the peak pressure P of the pulse1200MPa, pressure P of the edge of the spot2100MPa, 2 sigmaH≤P1≤2.5σH，P2≥σHWherein
(5) The grain distribution of the cross section obtained by linear cutting of the sample 2 along the thickness direction is shown in fig. 3, the microstructure of the neodymium iron boron is in gradient change, and the average grain size of the neodymium iron boron is gradually reduced from 3.5 mu m inside the sample to 1.5 mu m on the surface of the sample under the action of laser impact. The grain boundary volume of the surface layer is increased due to the reduction of the particle size, namely the content of diffused Dy is gradually reduced from the surface along the depth direction, and the average grain size of the infiltrated Dy is about 20-50 nm. Obviously, the microstructure change of neodymium iron boron caused by laser shock diffusion of Dy is reflected in two aspects on the magnetic property: firstly, the reduction of the size of the surface neodymium iron boron is beneficial to the increase of the coercive force of the system, and secondly, the intervention of a Dy rare earth crystal boundary strengthens the pinning effect of the system, so that the coercive force of the system is increased. The coercive force of the neodymium iron boron can be effectively improved under the combined action of the two aspects. The section coercive force is distributed along the depth of the sample as shown in figure 4, the coercive force is obviously reduced in gradient within 1mm, and is almost unchanged when the coercive force exceeds 1mm, which shows that the laser impact technology can form gradient change within 1mm of the surface layer of the neodymium iron boron, the diffusion depth is obviously greater than that of the conventional diffusion technology, and the coercive force is increased by more than 50% compared with that of the sample 1.
Claims (7)
1. A preparation method of a sintered neodymium iron boron magnet surface layer magnetic gradient nano structure is characterized by comprising the following steps: firstly, soaking a sintered neodymium-iron-boron magnet in a chlorine-containing solution for a period of time, expanding a grain boundary gap after a grain boundary on the surface layer of the sintered neodymium-iron-boron magnet is corroded, cleaning the surface of the sintered neodymium-iron-boron magnet after corrosion treatment, and then implanting magnetic rare earth metal nano powder into the expanded grain boundary after corrosion through the force effect of laser shock waves by adopting a laser shock strengthening technology, so that a magnetic gradient nano structure is obtained on the surface layer of the sintered neodymium-iron-boron magnet;
the corrosion treatment process of the chlorine-containing solution comprises the following steps: preparing a NaCl solution with the solute mass fraction of 5-20% at normal temperature, and immersing the sintered neodymium-iron-boron magnet into the prepared NaCl solution for corrosion for 30-60 min;
in the laser shock implantation treatment process, the laser process parameters are as follows: the pulse width is 8-30 ns, the pulse energy is 2-10J, the frequency is 1Hz, the diameter of a light spot is 2-3 mm, the number of impact layers is 1-3, a restraint layer is a water film with the thickness of 1-2 mm formed by deionized water flow, and the peak pressure of the pulse is P1Pressure at the edge of the light spot is P2Satisfies 2 sigmaH≤P1≤2.5σH，P2≥σHWherein
In the formula (I), the compound is shown in the specification,
and v is the Poisson's ratio of the material, so that the whole laser impact light spot area generates dynamic plastic deformation, and the metal workpiece in the light spot central area does not generate macroscopic deformation.
2. The method for preparing the surface magnetic gradient nanostructure of the sintered nd-fe-b magnet as claimed in claim 1, wherein the magnetic rare earth metal nanopowder is Dy nanopowder or Tb nanopowder.
3. The method for preparing the surface magnetic gradient nanostructure of the sintered neodymium-iron-boron magnet according to claim 1, wherein the cleaning process comprises the following steps: the surface of the sintered neodymium-iron-boron magnet is washed by deionized water, and then the sintered neodymium-iron-boron magnet is ultrasonically cleaned by the deionized water, so that chlorine-containing solution and corrosion products in a crystal boundary are removed.
4. The method for preparing the surface magnetic gradient nanostructure of the sintered neodymium-iron-boron magnet according to claim 1, wherein the laser shock implantation treatment process comprises the following steps: and adhering a composite absorption layer consisting of a laser absorption layer and a magnetic rare earth metal nano powder layer to a to-be-impacted area on the surface of the sintered neodymium-iron-boron magnet, wherein the composite absorption layer absorbs laser energy to generate plasma shock waves, and under the action of high-pressure impact force, the unvaporized magnetic rare earth metal nano powder particles are implanted into the surface layer of the sintered neodymium-iron-boron magnet.
5. The method for preparing the surface magnetic gradient nanostructure of the sintered NdFeB magnet as claimed in claim 4, wherein the composite absorption layer is composed of two parts: the first layer is a laser absorption layer with the thickness of 0.1mm and used for absorbing laser energy, and the laser absorption layer is a special aluminum foil for laser shock strengthening produced by American 3M company; the second layer is a magnetic rare earth metal nano powder layer with the thickness of 0.1-0.2 mm, and is used for providing nano powder mask particles implanted into the surface layer of the sintered neodymium-iron-boron magnet, and the second layer comprises the following components in percentage by mass: 80 wt% of magnetic rare earth metal nano powder, 15 wt% of high-temperature sealant and 5 wt% of additive for improving the flexibility of a rare earth metal nano powder particle layer; the second layer is coated on the first layer.
6. The method for preparing the surface magnetic gradient nanostructure of the sintered neodymium-iron-boron magnet as claimed in claim 5, wherein the additive for improving the flexibility of the magnetic rare earth metal nano powder particle layer is: the method comprises the following steps of mixing thinner, glyceride, phthalic anhydride and sebacic acid in a mass ratio of 2: 2: 1: 1, uniformly mixing to prepare the flexible polyester material.
7. The method for preparing the surface magnetic gradient nanostructure of the sintered NdFeB magnet as claimed in claim 4, wherein the preparation process of the composite absorption layer is as follows: uniformly mixing magnetic rare earth metal nano powder, high-temperature sealant and an additive in proportion, coating the mixture on a laser absorption layer, placing the composite absorption layer consisting of the laser absorption layer and the magnetic rare earth metal nano powder layer in a vacuum environment to remove bubbles, then placing the composite absorption layer in a mold, heating to 70-90 ℃, taking out the composite absorption layer from the mold after cooling, and carrying out vacuum plastic package for later use.
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| CN110473684B (en) * | 2019-08-19 | 2020-09-01 | 中国计量大学 | Preparation method of high-coercivity sintered neodymium-iron-boron magnet |
| CN110556243B (en) * | 2019-08-19 | 2021-07-02 | 安徽省瀚海新材料股份有限公司 | Neodymium iron boron surface dysprosium penetration method |
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