WO2021017967A1 - 一种稀土永磁材料及其原料组合物、制备方法和应用 - Google Patents
一种稀土永磁材料及其原料组合物、制备方法和应用 Download PDFInfo
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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
- H01F41/0293—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 diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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Definitions
- the invention relates to a rare earth permanent magnet material and its raw material composition, preparation method and application.
- R-T-B series rare earth permanent magnet materials have been widely used in modern industry and electronic technology, such as electronic computers, automatic control systems, motors and generators, nuclear magnetic resonance imagers, audio devices, material edge devices, communication equipment and many other fields. With the development of new application fields and the harsh and changeable application conditions, the demand for products with high coercivity is increasing.
- Hcj intrinsic coercivity
- Nd forms DyFeB or TbFeB.
- Br residual magnetic flux density
- the sintering temperature is lower and the sintering compactness is poor, resulting in the low Br of the permanent magnet material; for example, it can be used in the RTB rare earth permanent Ti is added to the formulation of the magnetic material to increase the Hcj of the magnet, but this formulation is easy to form a high melting point rich Ti phase, which leads to the deterioration of the grain boundary diffusion effect, which is not conducive to the improvement of the Hcj of the magnet.
- the technical problem to be solved by the present invention is to overcome the defect that Br and Hcj of the R-T-B rare earth permanent magnet material in the prior art are difficult to achieve synchronous improvement, and provide a rare earth permanent magnet material and its raw material composition, preparation method and application.
- the R-T-B system permanent magnet material in the present invention has excellent performance, Br ⁇ 14.30kGs, Hcj ⁇ 24.1kOe, and realizes the synchronous improvement of Br and Hcj.
- the RTB-based permanent magnet material of the present invention is added with ⁇ 0.30wt.% Cu and 0.05-0.20wt.% Ti. Part of Ti enters the grain boundary to form high Cu-rich Ti phases. It can be completely dissolved in the grain boundary diffusion, which is beneficial to the grain boundary diffusion, and the Hcj is greatly improved.
- the present invention provides a R-T-B series permanent magnet material, which comprises the following components in terms of mass percentage:
- R 29.0-32.0wt.%, and R includes RH, and the content of the RH>1wt.%;
- the balance is Fe and unavoidable impurities; among them:
- the R is a rare earth element, and the R includes at least Nd;
- the RH is a heavy rare earth element, and the RH includes at least Tb.
- the R may also include rare earth elements conventional in the art, such as Pr.
- the content of R is preferably 29.5-32.0wt.%, such as 30.05wt.%, 31.05wt.%, 31.06wt.%, 31.07wt.%, 31.3wt.%, or 31.56wt.%, wt.% refers to the mass percentage in the RTB-based permanent magnetic material.
- the RH may also include heavy rare earth elements conventional in the art, such as Dy.
- the content of the RH is preferably 1.05-1.30wt.%, such as 1.05wt.%, 1.06wt.%, 1.07wt.% or 1.30wt.%, and wt.% refers to the RH in the RTB system.
- the mass percentage in the magnetic material is preferably 1.05-1.30wt.%, such as 1.05wt.%, 1.06wt.%, 1.07wt.% or 1.30wt.%, and wt.% refers to the RH in the RTB system.
- the mass percentage in the magnetic material is preferably 1.05-1.30wt.%, such as 1.05wt.%, 1.06wt.%, 1.07wt.% or 1.30wt.%.
- the RH also includes Dy
- the Tb content is 0.5 wt.%
- the Dy content is 0.8 wt.%
- wt.% refers to the content in the RTB-based permanent magnetic material Mass percentage.
- the content of Cu is preferably 0.30-0.45wt.%, such as 0.30wt.%, 0.35wt.%, 0.40wt.% or 0.45wt.%, and wt.% refers to the permanent The mass percentage in the magnetic material.
- the content of Co is preferably 0.10wt.% or 0.50-1.0wt.%, such as 0.50wt.%, 0.80wt.% or 1.0wt.%, and wt.% refers to the permanent The mass percentage in the magnetic material.
- the content of Ti is preferably 0.05wt.% or 0.10-0.20wt.%, such as 0.10wt.%, 0.15wt.% or 0.20wt.%, and wt.% refers to the permanent The mass percentage in the magnetic material.
- the content of B is preferably 0.92-0.96wt.% or 0.94-0.98wt.%, such as 0.92wt.%, 0.94wt.%, 0.95wt.% or 0.98wt.%, and wt.% is Refers to the mass percentage in the RTB-based permanent magnet material.
- the R-T-B series permanent magnetic material includes the following components:
- R 29.5-32.0wt.%, the content of the RH is 1.05-1.3wt.%;
- wt.% refers to the mass percentage in the R-T-B-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 29.0wt.%, Tb is 1.05wt.%, Cu is 0.30wt.%, and Co is 0.10wt.% , Ti is 0.05wt.% and B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 1.05wt.%, Cu is 0.30wt.%, and Co is 0.10wt.% , Ti is 0.05wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.5wt.%, Tb is 1.06wt.%, Cu is 0.30wt.%, and Co is 0.10wt.% , Ti is 0.05wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 1.05wt.%, Cu is 0.35wt.%, and Co is 0.50wt.% , Ti is 0.10wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 1.07wt.%, Cu is 0.40wt.%, and Co is 0.50wt.% , Ti is 0.10wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 1.06wt.%, Cu is 0.45wt.%, and Co is 0.50wt.% , Ti is 0.10wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 1.06wt.%, Cu is 0.40wt.%, and Co is 0.8wt.% , Ti is 0.10wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnetic material includes the following components: Nd is 30.0wt.%, Tb is 1.07wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.05wt.%, B is 0.94wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 1.06wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.10wt.%, B is 0.94wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnetic material includes the following components: Nd is 30.0wt.%, Tb is 1.05wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.15wt.%, B is 0.94wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnetic material includes the following components: Nd is 30.0wt.%, Tb is 1.05wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.20wt.%, B is 0.94wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 1.06wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.10wt.%, B is 0.95wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnetic material includes the following components: Nd is 30.0wt.%, Tb is 1.05wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.10wt.%, B is 0.98wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: PrNd is 30wt.%, Tb is 0.5wt.%, Dy is 0.8wt.%, Cu is 0.40wt.%, Co is 0.5wt.%, Ti is 0.1wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the RTB-based permanent magnetic material.
- the RTB-based permanent magnetic material has a high Cu and high Ti phase with a composition ratio of (T 1-ab -Ti a -Cu b ) x -R y at the grain boundaries of the magnet; wherein: T represents Fe and Co , 1.5b ⁇ a ⁇ 2b, 70at% ⁇ x ⁇ 82at%, 18at% ⁇ y ⁇ 30at%.
- At% refers to atomic percentage, and specifically refers to the percentage of atomic content of various elements in the R-T-B permanent magnetic material.
- the a may be 2.50-3.0 at%.
- the y may be 20.0-23.0 at%.
- the present invention also provides a raw material composition of R-T-B series permanent magnet material, which includes the following components in terms of mass percentage:
- R 29.0-31.5wt.%, and R includes RH, and the content of the RH is 0.1-0.9wt.%;
- the balance is Fe and unavoidable impurities; among them:
- the R is a rare earth element, and the R includes at least Nd;
- the RH is a heavy rare earth element.
- the R may also include rare earth elements conventional in the art, such as Pr.
- the content of R is preferably 29.5-31.0wt.%, such as 29.5wt.%, 30.5wt.%, 30.8wt.% or 31.0wt.%, and wt.% means that the RTB The mass percentage in the raw material composition of the magnetic material.
- the RH may be a conventional heavy rare earth element such as Tb and/or Dy.
- the RH content is preferably 0.5-0.9wt.%, such as 0.5wt.% or 0.8wt.%, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material .
- the content of Cu is preferably 0.30-0.45wt.%, such as 0.30wt.%, 0.35wt.%, 0.40wt.% or 0.45wt.%, and wt.% refers to the permanent The mass percentage in the raw material composition of the magnetic material.
- the content of Co is preferably 0.10wt.% or 0.50-1.0wt.%, such as 0.50wt.%, 0.80wt.% or 1.0wt.%, and wt.% refers to the permanent The mass percentage in the raw material composition of the magnetic material.
- the content of Ti is preferably 0.05wt.% or 0.10-0.20wt.%, such as 0.10wt.%, 0.15wt.% or 0.20wt.%, and wt.% refers to the permanent The mass percentage in the raw material composition of the magnetic material.
- the content of B is preferably 0.92-0.96wt.% or 0.94-0.98wt.%, such as 0.92wt.%, 0.94wt.%, 0.95wt.% or 0.98wt.%, and wt.% is Refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the raw material composition of the R-T-B permanent magnet material includes the following components:
- the wt.% refers to the mass percentage in the raw material composition of the R-T-B permanent magnetic material.
- the RTB-based permanent magnet material includes the following components: Nd is 29.0wt.%, Tb is 0.50wt.%, Cu is 0.30wt.%, and Co is 0.10wt.% , Ti is 0.05wt.% and B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.30wt.%, and Co is 0.10wt.% , Ti is 0.05wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.5wt.%, Tb is 0.50wt.%, Cu is 0.30wt.%, and Co is 0.10wt.% , Ti is 0.05wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.35wt.%, and Co is 0.50wt.% , Ti is 0.10wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.40wt.%, and Co is 0.50wt.% , Ti is 0.10wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.45wt.%, and Co is 0.50wt.% , Ti is 0.10wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.40wt.%, and Co is 0.8wt.% , Ti is 0.10wt.%, B is 0.92wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.05wt.%, B is 0.94wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.10wt.%, B is 0.94wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.15 wt.%, B is 0.94 wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.20wt.%, B is 0.94wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.10 wt.%, B is 0.95 wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: Nd is 30.0wt.%, Tb is 0.50wt.%, Cu is 0.40wt.%, and Co is 1.0wt.% , Ti is 0.10 wt.%, B is 0.98 wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the RTB-based permanent magnetic material includes the following components: PrNd is 30wt.%, Dy is 0.8wt.%, Cu is 0.40wt.%, Co is 0.5wt.%, Ti is 0.1 wt.%, B is 0.92 wt.%, the balance is Fe, and wt.% refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the present invention also provides a method for preparing an RTB-based permanent magnet material, which includes the following steps: casting, crushing, crushing, forming, sintering and grain boundary molten liquid of the raw material composition of the RTB-based permanent magnet material Diffusion treatment to obtain the RTB-based permanent magnet material;
- the heavy rare earth element in the grain boundary diffusion treatment includes Tb.
- the molten liquid of the raw material composition of the RTB-based permanent magnet material can be prepared according to a conventional method in the art, for example, smelting in a high-frequency vacuum induction melting furnace.
- the vacuum degree of the smelting furnace may be 5 ⁇ 10 -2 Pa.
- the melting temperature may be 1500°C or less.
- the casting process can be a conventional casting process in the field, for example: in an Ar gas atmosphere (for example, under an Ar gas atmosphere of 5.5 ⁇ 10 4 Pa), at 10 2 °C/sec-10 4 °C/ Cool down at a rate of seconds, that's it.
- an Ar gas atmosphere for example, under an Ar gas atmosphere of 5.5 ⁇ 10 4 Pa
- 10 2 °C/sec-10 4 °C/ Cool down at a rate of seconds, that's it.
- the crushing process can be a conventional crushing process in the field, such as hydrogen absorption, dehydrogenation, and cooling treatment.
- the hydrogen absorption can be performed under the condition of a hydrogen pressure of 0.15 MPa.
- the dehydrogenation can be carried out under the condition of raising the temperature while drawing a vacuum.
- the pulverization process can be a conventional pulverization process in the field, such as jet mill pulverization.
- the jet mill pulverization can be performed in a nitrogen atmosphere with an oxidizing gas content of 150 ppm or less.
- the oxidizing gas refers to oxygen or moisture content.
- the pressure of the crushing chamber of the jet mill crushing may be 0.38 MPa.
- the pulverization time of the jet mill may be 3 hours.
- a lubricant such as zinc stearate
- the added amount of the lubricant may be 0.10-0.15% of the weight of the powder after mixing, for example 0.12%.
- the forming process may be a conventional forming process in the field, such as a magnetic field forming method or a hot pressing and thermal deformation method.
- the sintering process can be a conventional sintering process in the field, for example, preheating, sintering, and cooling under vacuum conditions (for example, under a vacuum of 5 ⁇ 10 -3 Pa).
- the preheating temperature may be 300-600°C.
- the preheating time can be 1-2h.
- the preheating is for 1 hour at a temperature of 300°C and 600°C each.
- the sintering temperature may be a conventional sintering temperature in the art, for example, 900°C to 1100°C, and for example, 1040°C.
- the sintering time may be a conventional sintering time in the field, for example, 2h.
- Ar gas can be introduced before cooling to make the gas pressure reach 0.1 MPa.
- the grain boundary diffusion treatment can be processed according to conventional processes in the field, for example, the surface of the RTB-based permanent magnet material is vapor-deposited, coated or sputtered to attach a substance containing Tb, and then subjected to diffusion heat treatment, That's it.
- the material containing Tb may be Tb metal, a compound or alloy containing Tb.
- the temperature of the diffusion heat treatment may be 800-900°C, such as 850°C.
- the time of the diffusion heat treatment may be 12-48h, such as 24h.
- heat treatment may also be performed.
- the temperature of the heat treatment may be 450-550°C, for example 500°C.
- the heat treatment time may be 3h.
- the invention also provides an R-T-B series permanent magnet material prepared by the above method.
- the invention also provides an application of the R-T-B series permanent magnet material as an electronic component in a motor.
- the application can be used as an electronic component in a motor with a motor speed of 3000-7000rpm and/or a motor operating temperature of 80-180°C, and can also be used as an electronic component in a high-speed motor and/or household appliances. Device use.
- the high-speed motor generally refers to a motor whose speed exceeds 10000 r/min.
- the home appliance may be an inverter air conditioner.
- the reagents and raw materials used in the present invention are all commercially available.
- the R-T-B series permanent magnet material of the present invention has excellent performance, Br ⁇ 14.30kGs, Hcj ⁇ 24.1kOe, and realizes the synchronous improvement of Br and Hcj.
- the RTB-based permanent magnet material of the present invention is added with ⁇ 0.30wt.% Cu and 0.05-0.20wt.% Ti. Part of Ti enters the grain boundary to form a high Cu-rich Ti phase. These phases can be completely dissolved in the grain boundary diffusion, which is beneficial to the grain boundary diffusion, and the Hcj is greatly improved.
- Figure 1 is the Nd, Cu, and Ti distribution diagrams of the permanent magnetic material prepared in Example 7 formed by scanning the FE-EPMA surface (from left to right are the concentration distribution diagrams of Nd, Cu, and Ti elements, the legend shows the difference The colors correspond to different concentration values), in which point 1 is the main phase and point 2 is the high Cu-rich Ti phase.
- Fig. 2 is a distribution diagram of Nd, Cu, and Ti formed by scanning the permanent magnetic material FE-EPMA prepared in Comparative Example 3.
- the purity of Nd and Tb is 99.8%
- the purity of Fe-B is technical grade purity
- the purity of pure Fe is technical grade purity
- the purity of Co, Cu, and Ti is 99.9%.
- R-T-B permanent magnetic materials in the examples and comparative examples are shown in Table 1.
- wt.% refers to the mass percentage of each raw material in the R-T-B-based permanent magnetic material, and "/" means that the element is not added.
- Example 1 29.0 / 0.50 / 0.30 0.10 0.05 0.92 margin / / / / / Example 2 30.0 / 0.50 / 0.30 0.10 0.05 0.92 margin / / / / / Example 3 30.5 / 0.50 / 0.30 0.10 0.05 0.92 margin / / / / / Example 4 30.0 / 0.50 / 0.35 0.50 0.10 0.92 margin / / / / / / Example 5 30.0 / 0.50 / 0.40 0.50 0.10 0.92 margin / / / / / / Example 6 30.0 / 0.50 / 0.45 0.50 0.10 0.92 margin / / / / / / Example 7 30.0 / 0.50 / 0.40 0.80 0.10 0.92 margin / / / / / / Example 8 30.0 / 0.50 / 0.40 1.0
- R-T-B series permanent magnet material The preparation method of R-T-B series permanent magnet material is as follows:
- Hydrogen breaking and pulverizing process vacuum the hydrogen breaking furnace containing the quench alloy at room temperature, and then inject hydrogen with a purity of 99.9% into the hydrogen breaking furnace to maintain the hydrogen pressure at 0.15MPa; after fully absorbing hydrogen, The temperature is raised while vacuuming, and the hydrogen is fully dehydrogenated; then the cooling is performed, and the powder after the hydrogen breakage is taken out.
- Fine pulverization step under a nitrogen atmosphere with an oxidizing gas content of 150 ppm or less and a pulverization chamber pressure of 0.38 MPa, the powder after hydrogen pulverization is jet milled for 3 hours to obtain a fine powder.
- Oxidizing gas refers to oxygen or moisture.
- Magnetic field forming process using a right-angle orientation type magnetic field forming machine, in a 1.6T orientation magnetic field and under a forming pressure of 0.35ton/cm 2 , the above-mentioned zinc stearate-added powder is formed into a side length at a time It is a 25mm cube; it is demagnetized in a 0.2T magnetic field after one-time forming.
- a secondary molding machine isostatic press
- each compact is moved to a sintering furnace for sintering, sintered under a vacuum of 5 ⁇ 10 -3 Pa and at a temperature of 300°C and 600°C, respectively, for 1 hour; then, at 1040°C The sintering temperature is 2 hours; then Ar gas is introduced to make the pressure reach 0.1MPa, and then cooled to room temperature.
- each group of sintered bodies are processed into magnets with a diameter of 20mm and a thickness of 5mm.
- the thickness direction is the direction of the magnetic field orientation.
- the raw materials made of Tb fluoride are used for spray coating.
- the coated magnet is dried, and the metal with Tb element is sputtered on the surface of the magnet in a high-purity Ar gas atmosphere, followed by diffusion heat treatment at a temperature of 850°C for 24 hours. Cool to room temperature.
- Magnetic performance evaluation Use the NIM-10000H BH bulk rare earth permanent magnet non-destructive measurement system of China Metrology Institute for magnetic performance testing. Table 2 below shows the magnetic performance test results.
- “Br” is the residual magnetic flux density
- “Hcj” is the intrinsic coercivity
- “SQ” is the squareness (squareness ratio)
- “BHmax” is the maximum energy product (maximum energy product).
- Example 1 14.51 24.4 99.0 51.0
- Example 2 14.42 25.1 99.6 50.3
- Example 3 14.32 25.6 99.6 49.6
- Example 4 14.49 24.3 99.5 50.8
- Example 5 14.41 25.2 99.7 50.5
- Example 6 14.33 24.1 99.8 49.6
- Example 7 14.45 25.5 99.8 50.3
- Example 8 14.48 24.9 99.6 50.6
- Example 9 14.50 24.5 99.4 51.0
- Example 10 14.49 24.5 99.5 50.7
- Example 11 14.45 24.9 99.2 50.6
- Example 12 14.39 25.2 99.1 50.1
- Example 13 14.42 24.3 99.5 50.6
- Example 14 14.30 25.7 99.5 49.7 Comparative example 1 14.06 16.8 88.2 47.0 Comparative example 2 13.24 26.1 99.0 42.1 Comparative example 3 14.52 21.6 99.3 51.0 Comparative example 4 14.24 23.4 97.6 49.1 Comparative example 5 14.21 23.2 99.0 48.9 Comparative example 6 14.
- R-T-B series permanent magnet material in this application has excellent performance, Br ⁇ 14.30kGs, Hcj ⁇ 24.1kOe, which realizes the simultaneous improvement of Br and Hcj (Embodiment 1-14);
- Example 1 29.0 / 1.05 / 0.30 0.10 0.05 0.92 margin / / / / / Example 2 30.0 / 1.05 / 0.30 0.10 0.05 0.92 margin / / / / / Example 3 30.5 / 1.06 / 0.30 0.10 0.05 0.92 margin / / / / / Example 4 30.0 / 1.05 / 0.35 0.50 0.10 0.92 margin / / / / / / Example 5 30.0 / 1.07 / 0.40 0.50 0.10 0.92 margin / / / / / / Example 6 30.0 / 1.06 / 0.45 0.50 0.10 0.92 margin / / / / / / Example 7 30.0 / 1.06 / 0.40 0.8 0.10 0.92 margin / / / / / / Example 8 30.0 / 1.07 / 0.40 1.0
- FE-EPMA detection Polish the vertical orientation surface of the permanent magnet material, and use the field emission electron probe microanalyzer (FE-EPMA) (JEOL, 8530F) to detect. First, determine the distribution of Nd, Cu, Ti and other elements in the permanent magnetic material by scanning FE-EPMA, and then determine the content of Cu, Ti and other elements in the key phase by FE-EPMA single-point quantitative analysis.
- the test condition is the acceleration voltage of 15kv, Probe beam current is 50nA.
- Example 7 The permanent magnet material prepared in Example 7 was tested by FE-EPMA, and the results are shown in Table 4 and Figure 1 below. among them:
- Figure 1 shows the concentration profiles of Nd, Cu, and Ti respectively. It can be seen from Figure 1 that apart from being dispersedly distributed in the main phase, Ti-rich phases also exist at the grain boundaries. The Cu content in the Ti-rich phase is also higher than the main phase. In Figure 1, point 1 is the main phase and point 2 is the Ti-rich phase.
- Table 4 shows the results of FE-EPMA single-point quantitative analysis of the Ti-rich phase in FIG. 1. It can be seen from Table 4 that in the Ti-rich phase, the Ti content is 1.8 atomic ratios of the Cu content, and the rare earth content is about 21.3 at%. In the same way, the FE-EPMA test of other examples shows that there are high Cu and high Ti phases at the grain boundaries. The Ti content is 1.5-2 times the atomic ratio of Cu, and the total rare earth is 18-30at% (At% refers to the atomic percentage, specifically refers to the percentage of the atomic content of various elements).
- the comparative example 3 was tested by FE-EPMA, and the results are shown in Fig. 2, which respectively represent the concentration distribution diagrams of Nd, Cu, and Ti. It can be seen from the results that Ti is dispersed in the main phase, and no high Cu and high Ti phases are formed at the grain boundaries. In testing other comparative examples, no high Cu and high Ti phases were observed in the grain boundaries of the permanent magnet materials.
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Abstract
Description
编号 | Nd | PrNd | Tb | Dy | Cu | Co | Ti | B | Fe | Ga | Al | Zr | Mo | W | Mn |
实施例1 | 29.0 | / | 0.50 | / | 0.30 | 0.10 | 0.05 | 0.92 | 余量 | / | / | / | / | / | / |
实施例2 | 30.0 | / | 0.50 | / | 0.30 | 0.10 | 0.05 | 0.92 | 余量 | / | / | / | / | / | / |
实施例3 | 30.5 | / | 0.50 | / | 0.30 | 0.10 | 0.05 | 0.92 | 余量 | / | / | / | / | / | / |
实施例4 | 30.0 | / | 0.50 | / | 0.35 | 0.50 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
实施例5 | 30.0 | / | 0.50 | / | 0.40 | 0.50 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
实施例6 | 30.0 | / | 0.50 | / | 0.45 | 0.50 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
实施例7 | 30.0 | / | 0.50 | / | 0.40 | 0.80 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
实施例8 | 30.0 | / | 0.50 | / | 0.40 | 1.0 | 0.05 | 0.94 | 余量 | / | / | / | / | / | / |
实施例9 | 30.0 | / | 0.50 | / | 0.40 | 1.0 | 0.10 | 0.94 | 余量 | / | / | / | / | / | / |
实施例10 | 30.0 | / | 0.50 | / | 0.40 | 1.0 | 0.15 | 0.94 | 余量 | / | / | / | / | / | / |
实施例11 | 30.0 | / | 0.50 | / | 0.40 | 1.0 | 0.20 | 0.94 | 余量 | / | / | / | / | / | / |
实施例12 | 30.0 | / | 0.50 | / | 0.40 | 1.0 | 0.10 | 0.95 | 余量 | / | / | / | / | / | / |
实施例13 | 30.0 | / | 0.50 | / | 0.40 | 1.0 | 0.10 | 0.98 | 余量 | / | / | / | / | / | / |
实施例14 | / | 30 | / | 0.8 | 0.4 | 0.5 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
对比例1 | 28.0 | / | 0.50 | / | 0.30 | 0.10 | 0.05 | 0.92 | 余量 | / | / | / | / | / | / |
对比例2 | 32.0 | / | 0.50 | / | 0.30 | 0.10 | 0.05 | 0.92 | 余量 | / | / | / | / | / | / |
对比例3 | 30.0 | / | 0.50 | / | 0.20 | 0.50 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
对比例4 | 30.0 | / | 0.50 | / | 0.50 | 0.50 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
对比例5 | 30.0 | / | 0.50 | / | 0.50 | 0.30 | 0.25 | 0.92 | 余量 | / | / | / | / | / | / |
对比例6 | 30.0 | / | 0.50 | / | 0.40 | 0.30 | 0.05 | 0.89 | 余量 | / | / | / | / | / | / |
对比例7 | 28.0 | / | 0.50 | / | 0.40 | 0.10 | 0.20 | 0.92 | 余量 | 0.30 | 0.20 | / | / | / | / |
对比例8 | 30.0 | / | 0.50 | / | 0.40 | 0.10 | / | 0.92 | 余量 | / | / | 0.20 | / | / | / |
对比例9 | 30.0 | / | 0.50 | / | 0.40 | 0.10 | / | 0.92 | 余量 | / | / | / | 0.20 | / | / |
对比例10 | 30.0 | / | 0.50 | / | 0.40 | 0.10 | / | 0.92 | 余量 | / | / | / | / | 0.20 | / |
对比例11 | / | 29.1 | / | 0.5 | 0.20 | 2.0 | / | 0.9 | 余量 | 0.20 | 0.20 | 0.15 | / | / | 0.03 |
编号 | Br(kGs) | Hcj(kOe) | SQ(%) | BHmax(MGoe) |
实施例1 | 14.51 | 24.4 | 99.0 | 51.0 |
实施例2 | 14.42 | 25.1 | 99.6 | 50.3 |
实施例3 | 14.32 | 25.6 | 99.6 | 49.6 |
实施例4 | 14.49 | 24.3 | 99.5 | 50.8 |
实施例5 | 14.41 | 25.2 | 99.7 | 50.5 |
实施例6 | 14.33 | 24.1 | 99.8 | 49.6 |
实施例7 | 14.45 | 25.5 | 99.8 | 50.3 |
实施例8 | 14.48 | 24.9 | 99.6 | 50.6 |
实施例9 | 14.50 | 24.5 | 99.4 | 51.0 |
实施例10 | 14.49 | 24.5 | 99.5 | 50.7 |
实施例11 | 14.45 | 24.9 | 99.2 | 50.6 |
实施例12 | 14.39 | 25.2 | 99.1 | 50.1 |
实施例13 | 14.42 | 24.3 | 99.5 | 50.6 |
实施例14 | 14.30 | 25.7 | 99.5 | 49.7 |
对比例1 | 14.06 | 16.8 | 88.2 | 47.0 |
对比例2 | 13.24 | 26.1 | 99.0 | 42.1 |
对比例3 | 14.52 | 21.6 | 99.3 | 51.0 |
对比例4 | 14.24 | 23.4 | 97.6 | 49.1 |
对比例5 | 14.21 | 23.2 | 99.0 | 48.9 |
对比例6 | 14.11 | 24.2 | 92.3 | 47.8 |
对比例7 | 13.84 | 25.5 | 99.0 | 46.4 |
对比例8 | 14.35 | 23.5 | 99.0 | 49.6 |
对比例9 | 14.25 | 23.2 | 98.9 | 49.0 |
对比例10 | 14.22 | 23.6 | 99.0 | 49.0 |
对比例11 | 14.28 | 25.9 | 91.6 | 48.3 |
编号 | Nd | PrNd | Tb | Dy | Cu | Co | Ti | B | Fe | Ga | Al | Zr | Mo | W | Mn |
实施例1 | 29.0 | / | 1.05 | / | 0.30 | 0.10 | 0.05 | 0.92 | 余量 | / | / | / | / | / | / |
实施例2 | 30.0 | / | 1.05 | / | 0.30 | 0.10 | 0.05 | 0.92 | 余量 | / | / | / | / | / | / |
实施例3 | 30.5 | / | 1.06 | / | 0.30 | 0.10 | 0.05 | 0.92 | 余量 | / | / | / | / | / | / |
实施例4 | 30.0 | / | 1.05 | / | 0.35 | 0.50 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
实施例5 | 30.0 | / | 1.07 | / | 0.40 | 0.50 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
实施例6 | 30.0 | / | 1.06 | / | 0.45 | 0.50 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
实施例7 | 30.0 | / | 1.06 | / | 0.40 | 0.8 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
实施例8 | 30.0 | / | 1.07 | / | 0.40 | 1.0 | 0.05 | 0.94 | 余量 | / | / | / | / | / | / |
实施例9 | 30.0 | / | 1.06 | / | 0.40 | 1.0 | 0.10 | 0.94 | 余量 | / | / | / | / | / | / |
实施例10 | 30.0 | / | 1.05 | / | 0.40 | 1.0 | 0.15 | 0.94 | 余量 | / | / | / | / | / | / |
实施例11 | 30.0 | / | 1.05 | / | 0.40 | 1.0 | 0.20 | 0.94 | 余量 | / | / | / | / | / | / |
实施例12 | 30.0 | / | 1.06 | / | 0.40 | 1.0 | 0.10 | 0.95 | 余量 | / | / | / | / | / | / |
实施例13 | 30.0 | / | 1.05 | / | 0.40 | 1.0 | 0.10 | 0.98 | 余量 | / | / | / | / | / | / |
实施例14 | / | 30 | 0.5 | 0.8 | 0.40 | 0.5 | 0.1 | 0.92 | 余量 | / | / | / | / | / | / |
对比例1 | 28.0 | / | 0.95 | / | 0.30 | 0.10 | 0.05 | 0.92 | 余量 | / | / | / | / | / | / |
对比例2 | 32.0 | / | 1.06 | / | 0.30 | 0.10 | 0.05 | 0.92 | 余量 | / | / | / | / | / | / |
对比例3 | 30.0 | / | 1.07 | / | 0.20 | 0.50 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
对比例4 | 30.0 | / | 1.05 | / | 0.50 | 0.50 | 0.10 | 0.92 | 余量 | / | / | / | / | / | / |
对比例5 | 30.0 | 1.03 | 0.5 | 0.30 | 0.25 | 0.92 | 余量 | / | / | / | / | / | / | ||
对比例6 | 30.0 | / | 1.06 | / | 0.40 | 0.30 | 0.05 | 0.89 | 余量 | / | / | / | / | / | / |
对比例7 | 28 | / | 1.07 | / | 0.40 | 0.10 | 0.20 | 0.92 | 余量 | 0.30 | 0.20 | / | / | / | / |
对比例8 | 30 | / | 1.06 | / | 0.40 | 0.10 | / | 0.92 | 余量 | / | / | 0.20 | / | / | / |
对比例9 | 30.0 | / | 1.07 | / | 0.40 | 0.10 | / | 0.92 | 余量 | / | / | / | 0.20 | / | / |
对比例10 | 30.0 | / | 1.06 | / | 0.40 | 0.10 | / | 0.92 | 余量 | / | / | / | / | 0.20 | / |
对比例11 | / | 29.1 | 0.35 | 0.5 | 0.20 | 2.0 | / | 0.9 | 余量 | 0.20 | 0.20 | 0.15 | / | / | 0.03 |
(at%) | Nd | Tb | Fe | Co | Cu | Ti | B | 相成分 |
点1 | 11.4 | 0.2 | 80.6 | 1.03 | 0.06 | 0.02 | 5.90 | R 2T 14B |
点2 | 18.0 | 3.2 | 73.2 | 0.98 | 1.48 | 2.72 | 0.33 | 高Cu高Ti相 |
Claims (10)
- 一种R-T-B系永磁材料,其特征在于,以质量百分比计,其包括下述组分:R:29.0-32.0wt.%,且R中包括RH,所述RH的含量>1wt.%;Cu:0.30-0.50wt.%,不包括0.50wt.%;Co:0.10-1.0wt.%;Ti:0.05-0.20wt.%;B:0.92-0.98wt.%;余量为Fe及不可避免的杂质;其中:所述R为稀土元素,所述R中至少包括Nd;所述RH为重稀土元素,所述RH中至少包括Tb。
- 如权利要求1所述的R-T-B系永磁材料,其特征在于,所述R的含量为29.5-32.0wt.%,优选为30.05wt.%、31.05wt.%、31.06wt.%、31.07wt.%、31.3wt.%、或31.56wt.%,wt.%是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述RH中还包括Dy;和/或,所述RH的含量为1.05-1.30wt.%,优选为1.05wt.%、1.06wt.%、1.07wt.%或1.30wt.%,wt.%是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述Cu的含量为0.30-0.45wt.%,优选为0.30wt.%、0.35wt.%、0.40wt.%或0.45wt.%,wt.%是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述Co的含量为0.10wt.%或0.50-1.0wt.%,优选为0.50wt.%、0.80wt.%或1.0wt.%,wt.%是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述Ti的含量为0.05wt.%或0.10-0.20wt.%,优选为0.10wt.%、0.15wt.%或0.20wt.%,wt.%是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述B的含量为0.92-0.96wt.%或0.94-0.98wt.%,优选为0.92wt.%、0.94wt.%、0.95wt.%或0.98wt.%,wt.%是指在所述R-T-B系永磁材料中的质量百分比。
- 如权利要求1所述的R-T-B系永磁材料,其特征在于,所述R-T-B系永磁材料中包括下述组分:R:29.5-32.0wt.%,所述RH的含量为1.05-1.3wt.%;Cu:0.30-0.45wt.%;Co:0.50-1.0wt.%;Ti:0.10-0.20wt.%;B:0.92-0.96wt.%;wt.%是指在所述R-T-B系永磁材料中的质量百分比。
- 如权利要求1-3中任一项所述的R-T-B系永磁材料,其特征在于,所述R-T-B系永磁材料在磁体晶界处存在组成比为(T 1-a-b-Ti a-Cu b) x-R y的高Cu高Ti相;其中:T代表Fe和Co,1.5b<a<2b,70at%<x<82at%,18at%<y<30at%,at%是指所述R-T-B系永磁材料中各元素的原子含量所占百分比。
- 一种R-T-B系永磁材料的原料组合物,其特征在于,以质量百分比计,其包括下述组分:R:29.0-31.5wt.%,且R中包括RH,所述RH的含量为0.1-0.9wt.%;Cu:0.30-0.50wt.%,不包括0.50wt.%;Co:0.10-1.0wt.%;Ti:0.05-0.20wt.%;B:0.92-0.98wt.%;余量为Fe及不可避免的杂质;其中:所述R为稀土元素,所述R中至少包括Nd;所述RH为重稀土元素。
- 如权利要求5所述的R-T-B系永磁材料的原料组合物,其特征在于,所述R的含量为29.5-31.0wt.%,优选为29.5wt.%、30.5wt.%、30.8wt.%或31.0wt.%,wt.%是指在所述R-T-B系永磁材料的原料组合物中的质量百分比;和/或,所述RH中包括Tb和/或Dy;和/或,所述RH的含量为0.5-0.9wt.%,优选为0.5wt.%或0.8wt.%,wt.%是指在所述R-T-B系永磁材料的原料组合物中的质量百分比;和/或,所述Cu的含量为0.30-0.45wt.%,优选为0.30wt.%、0.35wt.%、0.40wt.%或0.45wt.%,wt.%是指在所述R-T-B系永磁材料的原料组合物中的质量百分比;和/或,所述Co的含量为0.10wt.%或0.50-1.0wt.%,优选为0.50wt.%、0.80wt.%或1.0wt.%,wt.%是指在所述R-T-B系永磁材料的原料组合物中的质量百分比;和/或,所述Ti的含量为0.05wt.%或0.10-0.20wt.%,优选为0.10wt.%、0.15wt.%或0.20wt.%,wt.%是指在所述R-T-B系永磁材料的原料组合物中的质量百分比;和/或,所述B的含量为0.92-0.96wt.%或0.94-0.98wt.%,优选为0.92wt.%、0.94wt.%、0.95wt.%或0.98wt.%,wt.%是指在所述R-T-B系永磁材料的原料组合物中的质量百分比;或者,所述R-T-B系永磁材料的原料组合物中包括下述组分:R:29.5-31.0wt.%,RH:0.5-0.9wt.%;Cu:0.30-0.45wt.%;Co:0.50-1.0wt.%;Ti:0.10-0.20wt.%;B:0.92-0.96wt.%;wt.%是指在所述R-T-B系永磁材料的原料组合物中的质量百分比。
- 一种R-T-B系永磁材料的制备方法,其特征在于,其包括下述步骤:将如权利要求5或6所述的R-T-B系永磁材料的原料组合物的熔融液经铸造、破碎、粉碎、成形、烧结和晶界扩散处理,即得所述R-T-B系永磁材料;其中:所述晶界扩散处理中的重稀土元素包括Tb。
- 如权利要求7所述的R-T-B系永磁材料的制备方法,其特征在于,所述R-T-B系永磁材料的原料组合物的熔融液按下述方法制得:在高频真空感应熔炼炉中熔炼,即可;所述熔炼炉的真空度优选为5×10 -2Pa;所述熔炼的温度优选为1500℃以下;和/或,所述铸造的工艺按下述步骤进行:在Ar气气氛中,以10 2℃/秒-10 4℃/秒的速度冷却,即可;和/或,所述破碎的工艺按下述步骤进行:经吸氢、脱氢、冷却处理,即可;所述吸氢优选在氢气压力0.15MPa的条件下进行;所述粉碎优选为气流磨粉碎,所述气流磨粉碎的粉碎室压力优选为0.38MPa,所述气流磨粉碎的时间优选为3小时;和/或,所述成形的方法为磁场成形法或热压热变形法;和/或,所述烧结的工艺按下述步骤进行:在真空条件下,经预热、烧结、冷却,即可;所述预热的温度优选为300-600℃,所述预热的时间优选为1-2h;所述烧结的温度优选为900℃-1100℃,所述烧结的时间优选为2h;和/或,所述晶界扩散处理按下述步骤进行:在所述R-T-B系永磁材料的表面蒸镀、涂覆或溅射附着含有Tb的物质,经扩散热处理,即可;所述含有Tb的物质为Tb金属、含 有Tb的化合物或合金,所述扩散热处理的温度优选为800-900℃,所述扩散热处理的时间优选为12-48h;和/或,所述晶界扩散处理后,还进行热处理,所述热处理的温度优选为450-550℃,所述热处理的时间优选为3h。
- 一种如权利要求7或8中所述的R-T-B系永磁材料的制备方法制得的R-T-B系永磁材料。
- 一种如权利要求1-4、9中任一项所述R-T-B系永磁材料在马达中作为电子元器件的应用;所述应用优选为在3000-7000rpm电机转速和/或80-180℃电机工作温度的马达中作为电子元器件的应用;或者,在高转速电机和/或家电制品中作为电子元器件的应用。
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