WO2021128801A1 - 一种r-t-b系永磁材料及其制备方法和应用 - Google Patents
一种r-t-b系永磁材料及其制备方法和应用 Download PDFInfo
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- 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
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Definitions
- the invention relates to an R-T-B series permanent magnet material and a preparation method and application thereof.
- the current phase composed of PrNd (the mass ratio of Pr and Nd is 20:80 or 25 :75) It has been used in the commercial production of sintered permanent magnets. Due to its advantages of high magnetic energy product and high remanence, it has been used in motors, electro-acoustic devices, computer hard disk drives (HDD), military equipment, and human nuclear magnetic resonance. Imagers (MRI), microwave communication technology, controllers, meters, etc. have been widely used.
- PrNd the mass ratio of Pr and Nd is 20:80 or 25 :75
- Nd-Fe-B With the advancement of science and technology, higher requirements have been put forward for the performance of Nd-Fe-B. Many researchers have achieved the improvement of the performance of NdFeB materials by adding a large amount of heavy rare earth Dy or Tb, but excessive use Heavy rare earths will increase the cost of materials sharply, while the resources of heavy rare earths are relatively small.
- NdFeB magnets will inevitably introduce carbon, sulfur, hydrogen, oxygen, nitrogen and other impurity elements during the process, which poses no small challenge to the production of magnets with uniform and stable magnetic properties.
- a high carbon impurity content will cause the grain size of the main phase of the magnet and the distribution of the neodymium-rich phase to be uneven, causing various performance indexes of the magnet to decrease to varying degrees. Therefore, in order to improve the uniform stability of the magnet, strict control of the production process is required.
- the technical problem to be solved by the present invention is to overcome the defect that the performance improvement of sintered NdFeB magnets in the prior art is excessively dependent on heavy rare earth elements, and at the same time, the excessive content of carbon in the sintered NdFeB magnets will cause the performance of the magnet to decrease, and provide An RTB-based permanent magnet material and its preparation method and application are presented.
- the RTB-based permanent magnet material provided by the present invention can realize the improvement of the performance of the permanent magnet material under the condition of no heavy rare earth, and does not need to control the content of carbon element introduced in the process. Under the condition of high carbon element content, the magnet Still maintain excellent performance.
- the present invention provides a R-T-B series permanent magnet material, which comprises the following components in terms of mass percentage:
- R’ 29.5-33.5wt.%; wherein: the R’ is a rare earth element, the R’ includes Pr, and the content of the Pr is ⁇ 8.85wt.%;
- X 0-5.0wt.%, the X is one or more of Cu, Al, Ga, Co, Zr, Ti, Nb and Mn;
- the content of R' is preferably 29.5-33.4wt.%, such as 29.5wt.%, 30.5wt.%, 30.8wt.%, 31.0wt.%, 31.013wt.%, 31.075wt.%, 31.115wt.%, 31.5wt.%, 32.0wt.%, 32.3wt.%, 32.8wt.% or 33.3wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the content of Pr is preferably 8.85-27.15wt.%, more preferably ⁇ 17.00wt.%, such as 8.846wt.%, 8.848wt.%, 8.849wt.%, 8.851wt.%, 9.852wt. %, 10.148wt.%, 10.151wt.%, 10.848wt.%, 10.849wt.%, 11.848wt.%, 12.148wt.%, 12.15wt.%, 12.151wt.%, 13.149wt.%, 14.147wt.
- the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the R' may also include Nd and/or R, and the R is a rare earth element other than Pr and Nd.
- the Nd content is preferably 3.3-23.0wt.%, such as 3.348wt.%, 5.352wt.%, 6.652wt.%, 6.851wt.%, 7.351wt.%, 7.353wt.%, 7.849wt. %, 8.351wt.%, 8.651wt.%, 8.652wt.%, 8.852wt.%, 9.349wt.%, 9.352wt.%, 10.651wt.%, 10.851wt.%, 11.348wt.%, 11.351wt.
- the percentage refers to The mass percentage in the RTB-based permanent magnet material.
- the mass ratio of the Nd and the R' is preferably ⁇ 0.72, more preferably ⁇ 0.5, such as 0.110, 0.175, 0.216, 0.221, 0.233, 0.241, 0.253, 0.281, 0.283, 0.286, 0.297, 0.307, 0.317 , 0.346, 0.350, 0.360, 0.366, 0.372, 0.378, 0.382, 0.385, 0.392, 0.395, 0.411, 0.416, 0.422, 0.424, 0.438, 0.443, 0.447, 0.456, 0.470, 0.476, 0.479, 0.487, 0.520, 0.536, 0.541 , 0.544, 0.551, 0.554, 0.588, 0.598, 0.601, 0.606, 0.608, 0.614, 0.632, 0.644, 0.666, 0.671, 0.673, 0.678, 0.696, 0.697, 0.700, 0.710, 0.713
- the type of R is preferably Y and/or Ce.
- the content of R is preferably 0-1 wt.%, such as 0.29 wt.%, and the percentage refers to the mass percentage in the R-T-B series permanent magnetic material.
- the R' may also include heavy rare earth element RH.
- the type of RH may be Dy and/or Tb.
- the content of the RH may be a conventional content in the art, preferably 0.5-2.6wt.%, such as 0.58wt.%, 0.62wt.%, 1.212wt.%, 1.219wt.%, 1.51wt.%, 1.991wt.%, 2.011wt.%, 2.511wt.% or 2.512wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the mass ratio of the RH and the R is preferably ⁇ 0.253, such as 0.019-0.075, and further such as 0.019, 0.020, 0.038, 0.039, 0.047, 0.061 or 0.075.
- the content of Tb is preferably 0.5-2.0wt.%, such as 1.991wt.%, 1.212wt.%, 1.219wt.% or 0.58wt.%, and the percentage refers to the RTB is the mass percentage of permanent magnet materials.
- the content of Dy is preferably 0.6-2.52wt.%, such as 0.62wt.%, 1.51wt.%, 2.011wt.%, 2.511wt.% or 2.512wt.%, percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the content of C is preferably 0.106-0.25wt.%, such as 0.1062wt.%, 0.1069wt.%, 0.1072wt.%, 0.1075wt.%, 0.1251wt.%, 0.1253wt.%, 0.1256 wt.%, 0.1532wt.%, 0.1534wt.%, 0.1537wt.%, 0.1759wt.%, 0.1761wt.%, 0.1764wt.%, 0.1835wt.%, 0.184wt.%, 0.1843wt.%, 0.1846 wt.%, 0.1965wt.%, 0.197wt.%, 0.1973wt.%, 0.2139wt.%, 0.2144wt.%, 0.2147wt.%, 0.2243wt.%, 0.2245wt.%, 0.2248wt.%, 0.2251 wt.%, 0.2379wt.% or 0.2456wt.
- the content of O is preferably ⁇ 0.0691wt.%, such as 0.0382wt.%, 0.0384wt.%, 0.039wt.%, 0.0391wt.%, 0.041wt.%, 0.0412wt.%, 0.0432wt.
- the percentage refers to the RTB-based permanent magnetic material The percentage of mass.
- the content of B is preferably 0.94-1.1wt.%, such as 0.946wt.%, 0.947wt.%, 0.948wt.%, 0.949wt.%, 0.951wt.%, 0.952wt.%, 0.958 wt.%, 0.961wt.%, 0.962wt.%, 0.981wt.%, 0.982wt.%, 0.985wt.%, 0.998wt.%, 1.008wt.%, 1.009wt.%, 1.01wt.%, 1.011 wt.% or 1.012wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnetic material.
- the content of Fe is preferably 61.4-69.3wt.%, for example 61.49wt.%, 61.60wt.%, 62.15wt.%, 62.19wt.%, 62.66wt.%, 62.91wt.%, 63.52 wt.%, 63.62wt.%, 63.66wt.%, 64.71wt.%, 65.85wt.%, 66.02wt.%, 66.15wt.%, 66.19wt.%, 66.22wt.%, 66.23wt.%, 66.30 wt.%, 66.37wt.%, 66.40wt.%, 66.44wt.%, 66.57wt.%, 66.66wt.%, 66.70wt.%, 66.72wt.%, 66.75wt.%, 66.82w
- the X can be Cu, Al, Ga, Co, Zr, Ti or Nb, and can also be "Cu and Al", “Ga and Mn", “Cu, Al and Ga”, “Cu, Al” , Ga and Zr", "Cu, Al, Ga and Co” or "Cu, Al, Ga, Zr and Co".
- the content of X is preferably 0-4.5wt.%, such as 0.021wt.%, 0.041wt.%, 0.101wt.%, 0.102wt.%, 0.201wt.%, 0.202wt.%, 0.251 wt.%, 0.301wt.%, 0.302wt.%, 0.351wt.%, 0.352wt.%, 0.362wt.%, 0.401wt.%, 0.421wt.%, 0.423wt.%, 0.451wt.%, 0.497 wt.%, 0.5wt.%, 0.501wt.%, 0.523wt.%, 0.526wt.%, 0.601wt.%, 0.602wt.%, 0.643wt.%, 0.673wt.%, 0.702wt.%, 0.704 wt.%, 0.743wt.%, 0.801wt.%, 0.803wt
- the content of Cu is preferably 0.2-0.51 wt.%, for example, 0.201 wt.%, 0.302 wt.%, 0.34 wt.%, 0.341 wt.%, 0.351 wt.%, 0.381 wt.%, 0.382wt.%, 0.4wt.%, 0.401wt.%, 0.402wt.%, 0.403wt.%, 0.41wt.%, 0.42wt.%, 0.421wt.%, 0.441wt.%, 0.451 wt.%, 0.5wt.%, 0.501wt.% or 0.502wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnetic material.
- the content of Al is preferably 0-0.81wt.%, but not 0, such as 0.01-0.03wt.% or 0.5-0.8wt.%, or for example 0.01wt.%, 0.021wt.%, 0.03wt.%, 0.041wt.%, 0.042wt.%, 0.101wt.%, 0.102wt.%, 0.103wt.%, 0.202wt.%, 0.298wt.%, 0.301wt.%, 0.302wt.%, 0.351wt.%, 0.401wt.%, 0.402wt.%, 0.403wt.%, 0.451wt.%, 0.497wt.%, 0.501wt.%, 0.502wt.%, 0.601wt.%, 0.602wt.%, 0.702wt.%, 0.801wt.%, 0.802wt.% or 0.81wt.%, the percentage refers to the mass
- the content of Ga is preferably 0.0-1.85wt.%, but not 0, more preferably 0.1-1.552wt.%, such as 0.102wt.%, 0.151wt.%, 0.202 wt.%, 0.251wt.%, 0.3wt.%, 0.301wt.%, 0.302wt.%, 0.399wt.%, 0.401wt.%, 0.42wt.%, 0.421wt.%, 0.501wt.%, 0.502 wt.%, 0.901wt.%, 1.402wt.% or 1.552wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnetic material.
- the content of Co is preferably 0.0-3.0wt.%, but not 0, more preferably 0.5-2.5wt.%, such as 0.5wt.%, 1.0wt.% or 2.5 wt.%, percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the content of Zr is preferably 0.25-0.35wt.%, such as 0.25wt.%, 0.30wt.% or 0.35wt.%, and the percentage refers to the RTB-based permanent magnet material The mass percentage in.
- the Nb content is preferably 0.25-0.35wt.%, such as 0.25wt.%, 0.30wt.% or 0.35wt.%, and the percentage refers to the RTB-based permanent magnet material The mass percentage in.
- the content of Mn is preferably 0.0-0.03 wt.%, but not 0, such as 0.01 wt.%, and the percentage refers to the mass percentage in the R-T-B series permanent magnetic material.
- the R-T-B-based permanent magnetic material may also include conventional additive elements M, such as one or more of Ni, Zn, Ag, In, Sn, Bi, V, Cr, Hf, Ta, and W.
- conventional additive elements M such as one or more of Ni, Zn, Ag, In, Sn, Bi, V, Cr, Hf, Ta, and W.
- the type of M is preferably Cr.
- the content of M is preferably 0-0.15 wt.%, but not 0, such as 0.05 wt.% or 0.12 wt.%, and the percentage refers to the mass percentage in the R-T-B series permanent magnetic material.
- the RTB-based permanent magnetic material may also contain nitrogen element N.
- the content of the N element ⁇ 0.05wt.%, such as 0.0182wt.%, 0.0187wt.%, 0.0223wt.%, 0.0228wt.%, 0.025wt.%, 0.0251wt.%, 0.0256wt.%, 0.0284wt.%, 0.0285wt.%, 0.029wt.%, 0.0301wt.%, 0.0302wt.%, 0.0307wt.%, 0.0341wt.%, 0.0342wt.%, 0.0347wt.%, 0.0366wt.%, 0.0371wt.%, 0.0372wt.%, 0.0375wt.%, 0.0378wt.%, 0.0397wt.%, 0.0398wt.%, 0.0401wt.%, 0.0404wt.%, 0.0436wt.%, 0.0439wt.%
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Cu: 0.2-0.51wt.%, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Al: 0-0.81wt.%, but not 0, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, the percentage means in the RTB-based permanent magnet material The percentage of mass.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Ga: 0.1-1.85wt.%, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Co: 0.0-3.0wt.%, but not 0, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, the percentage refers to the RTB-based permanent magnet material The percentage of mass.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Zr: 0.25-0.35wt.%, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Nb: 0.25-0.35wt.%, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Cu: 0.34-0.51wt.%, Al: 0-0.81wt.%, but not 0, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, percentages refer to The mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Cu: 0.34-0.51wt.%, Al: 0-0.81wt.%, but not 0, Ga: 0.1-0.5wt.%, B: 0.94-1.1wt.%, Fe: 61.4 -69.3wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnetic material.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Cu: 0.34-0.51wt.%, Al: 0.25-0.81wt.%, Ga: 0.1-0.42wt.%, Zr: 0.25-0.30wt.%, B: 0.94-1.1wt.% , Fe: 61.4-69.3wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Cu: 0.34-0.51wt.%, Al: 0.25-0.81wt.%, Ga: 0.1-0.41wt.%, Co: 0.0-3.0wt.%, Zr: 0.25-0.30wt.% , Cr: 0.05-0.12wt.%, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, RH: 0.5-2.6wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Cu: 0.34-0.51wt.%, Al: 0.25-0.81wt.%, Ga: 0.1-0.41wt.%, Co: 0.0-3.0wt.% , Zr: 0.25-0.30wt.%, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, the percentage refers to the mass percentage in the RTB-based permanent magnet material.
- the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, Ce: 0-1wt.%, RH: 0.5 -2.6wt.%, C: 0.106-0.25wt.%, O: ⁇ 0.07wt.%, Cu: 0.34-0.51wt.%, Al: 0.25-0.81wt.%, Ga: 0.1-0.41wt.%, Co: 0.0-3.0wt.%, Zr: 0.25-0.30wt.%, B: 0.94-1.1wt.%, Fe: 61.4-69.3wt.%, the percentage refers to the mass in the RTB-based permanent magnet material percentage.
- the R-T-B system permanent magnetic material generally includes a main phase, a grain boundary phase and an intercrystalline triangular region, wherein the intercrystalline triangular region is also called a rare earth-rich phase.
- the percentage of the volume of the intergranular triangular area to the sum of the volume of the main phase, the grain boundary phase and the intergranular triangular area is ⁇ 9.0%, such as 3.2%, 3.3%, 3. %, 4.6%, 4.8% or 5.3%.
- the content of rare earth elements in the intercrystalline triangle region is 84.35%-85.85%, such as 84.35%, 84.8%, 84.9%, 85%, 85.2%, 85.3%, 85.4% or 85.85%, and the percentage is Refers to the mass percentage of the total mass of the elements in the intercrystalline triangle region.
- the content of the O element in the intercrystalline triangle region is 13.25-14.8%, such as 13.25%, 13.7%, 14.2%, 14.3%, 14.4%, 14.5%, 14.6%, 14.7%, 14.75% Or 14.8%, the percentage refers to the mass percentage of the total mass of the elements in the intercrystalline triangle region.
- the content of Cu element in the intergranular triangle region is 0.6-0.9%, such as 0.6%, 0.8% or 0.9%, and the percentage refers to the The mass percentage of the total mass of the elements in the intercrystalline triangle area.
- the content of Ga element in the intercrystalline triangle region is 0.4-0.6%, for example, 0.4% or 0.6%, and the percentage refers to the proportion of the intercrystalline triangle region.
- the mass percentage of the total mass of the elements in the zone is 0.4-0.6%, for example, 0.4% or 0.6%, and the percentage refers to the proportion of the intercrystalline triangle region.
- the RTB-based permanent magnet material includes Cu and Ga
- the content of Cu element is 0.3-0.4%
- the content of Ga element is 0.5-0.6%, for example, 0.3% Cu in the intergranular triangle region.
- 0.6% Ga, 0.4% Cu, 0.4% Ga, 0.4% Cu, 0.5% Ga, or 0.4% Cu, 0.6% Ga the percentage refers to the mass percentage of the total mass of the elements in the intercrystalline triangle region.
- the present invention also provides a method for preparing an RTB-based permanent magnet material, which includes the following steps: casting, hydrogen breaking, and pulverizing the molten liquid of the raw material composition of the RTB-based permanent magnet material to obtain a powder; The powder and the dispersant are mixed, and then subjected to pressing, forming, sintering and aging treatment, and then:
- R’ 29.5-33.5wt.%; said R’ is a rare earth element, said R’ includes Pr, and the content of said Pr is ⁇ 8.85wt.%;
- X 0-5.0wt.%, the X is one or more of Cu, Al, Ga, Co, Zr, Ti, Nb and Mn;
- O in the crushing atmosphere is less than or equal to 60 ppm
- the dispersant contains C (carbon) element, and the mass percentage of the dispersant in the powder after mixing is 0.04-0.2%.
- the content of R' is preferably 29.5-33.3wt.%, more preferably 29.5wt.%, 30.5wt.%, 30.8wt.%, 31wt.%, 31.5wt.%, 32wt.%, 32.3wt.%, 32.8wt.% or 33.3wt.%, the percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the content of Pr is preferably 8.85-27.15wt.%, such as 8.85wt.%, 9.85wt.%, 10.15wt.%, 10.85wt.%, 11.85wt.%, 12.15wt.%, 13.15 wt.%, 14.15wt.%, 16.15wt.%, 17.15wt.%, 18.15wt.%, 19.15wt.%, 20.15wt.%, 21.15wt.%, 22.15wt.%, 23.15wt.%, 24.15 wt.%, 25.15wt.% or 27.15wt.%, the percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the R' may also include Nd and/or R, and the R is a rare earth element other than Pr and Nd.
- the Nd content is preferably 3.35-22.65wt.%, more preferably 3.35wt.%, 5.35wt.%, 6.65wt.%, 6.85wt.%, 7.35wt.%, 7.85wt.%, 8.35 wt.%, 8.65wt.%, 8.85wt.%, 9.35wt.%, 10.65wt.%, 10.85wt.%, 11.35wt.%, 11.65wt.%, 11.85wt.%, 12.35wt.%, 12.65 wt.%, 13.35wt.%, 13.65wt.%, 13.85wt.%, 14.35wt.%, 14.65wt.%, 14.85wt.%, 15.35wt.%, 16.35wt.%, 16.65wt.%, 16.85 wt.%, 17.35wt.%, 17.65wt.%, 18.35wt.%, 18.65wt.%, 18.85wt.%, 19.35wt.
- the mass ratio of the Nd and the R' is preferably ⁇ 0.72, for example, 0.11, 0.18, 0.22, 0.23, 0.24, 0.25, 0.28, 0.29, 0.30, 0.31, 0.32, 0.35, 0.36, 0.37, 0.38, 0.39 , 0.40, 0.41, 0.42, 0.44, 0.45, 0.46, 0.47, 0.48, 0.49, 0.52, 0.54, 0.55, 0.59, 0.60, 0.61, 0.63, 0.64, 0.67, 0.68, 0.70 or 0.72.
- the type of R is preferably Y and/or Ce.
- the content of R is preferably 0-1 wt.%, such as 0.3 wt.%, and the percentage refers to the mass percentage in the raw material composition of the R-T-B series permanent magnetic material.
- the R' may also include heavy rare earth element RH.
- the type of RH may be Dy and/or Tb.
- the content of the RH may be a conventional content in the art, preferably 1.2-2.5wt.%, such as 1.2wt.%, 1.5wt.%, 2wt.% or 2.5wt.%, the percentage refers to the The mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the mass ratio of the RH to the R' is preferably ⁇ 0.253, such as 0.038-0.075, and further such as 0.038, 0.039, 0.046, 0.061 or 0.075.
- the content of Tb is preferably 1.2-2.0wt.%, such as 1.2wt.% or 2.0wt.%, and the percentage refers to the raw material composition of the RTB-based permanent magnet material The percentage of mass.
- the content of Dy is preferably 1.5-2.5wt.%, such as 1.5wt.%, 2.0wt.% or 2.5wt.%, and the percentage refers to the RTB-based permanent magnet material The percentage of mass in the composition of raw materials.
- the content of B is preferably 0.95-1.1wt.%, such as 0.95wt.%, 0.96wt.%, 0.98wt.% or 1.01wt.%, and the percentage refers to the RTB-based permanent magnet material The percentage of mass in the composition of raw materials.
- the content of Fe is preferably 61.5-69.5wt.%, such as 61.79wt.%, 61.89wt.%, 62.44wt.%, 62.89wt.%, 63.24wt.%, 63.84wt.%, 63.87 wt.%, 63.94wt.%, 64.99wt.%, 66.19wt.%, 66.29wt.%, 66.47wt.%, 66.52wt.%, 66.55wt.%, 66.61wt.%, 66.69wt.%, 66.75 wt.%, 66.85wt.%, 66.97wt.%, 67.00wt.%, 67.02wt.%, 67.068wt.%, 67.13wt.%, 67.14wt.%, 67.19wt.%, 67.24wt.%,
- the X can be Cu, Al, Ga, Co, Zr, Ti or Nb, and can also be "Cu and Al", “Ga and Mn", “Cu, Al and Ga”, “Cu, Al” , Ga and Zr", "Cu, Al, Ga and Co” or "Cu, Al, Ga, Zr and Co".
- the content of X is preferably 0-4.5wt.%, such as 0.02wt.%, 0.042wt.%, 0.1wt.%, 0.2wt.%, 0.25wt.%, 0.3wt.%, 0.35 wt.%, 0.36wt.%, 0.4wt.%, 0.42wt.%, 0.422wt.%, 0.45wt.%, 0.5wt.%, 0.52wt.%, 0.522wt.%, 0.6wt.%, 0.64 wt.%, 0.67wt.%, 0.7wt.%, 0.74wt.%, 0.8wt.%, 0.87wt.%, 0.88wt.%, 0.89wt.%, 0.9wt.%, 0.94wt.%, 1.00 wt.%, 1.02wt.%, 1.1wt.%, 1.19wt.%, 1.27wt.%, 1.3wt.%, 1.4
- the content of Cu is preferably 0.2-0.5wt.%, for example 0.2wt.%, 0.3wt.%, 0.34wt.%, 0.35wt.%, 0.38wt.%, 0.4 wt.%, 0.42wt.%, 0.44wt.%, 0.45wt.% or 0.5wt.%, the percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the content of Al is preferably 0-0.8wt.%, but not 0, such as 0.01-0.03wt.% or 0.5-0.8wt.%, or for example 0.01wt.%, 0.02wt.%, 0.03wt.%, 0.042wt.%, 0.1wt.%, 0.2wt.%, 0.3wt.%, 0.35wt.%, 0.4wt.%, 0.45wt.%, 0.5wt.%, 0.6wt.%, 0.7wt.% or 0.8wt.%, the percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the content of Ga is preferably 0.0-1.85wt.%, but not 0, more preferably 0.1-1.55wt.%, such as 0.1wt.%, 0.15wt.%, 0.2 wt.%, 0.25wt.%, 0.3wt.%, 0.4wt.%, 0.42wt.%, 0.5wt.%, 0.9wt.%, 1.4wt.% or 1.55wt.%, the percentage refers to the The mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the content of Co is preferably 0.0-3.0wt.%, but not 0, more preferably 0.5-2.5wt.%, such as 0.5wt.%, 1.0wt.% or 2.5 wt.%, percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the content of Zr is preferably 0.25-0.35wt.%, such as 0.25wt.%, 0.30wt.% or 0.35wt.%, and the percentage refers to the RTB-based permanent magnet material The percentage of mass in the composition of raw materials.
- the Nb content is preferably 0.25-0.35wt.%, such as 0.25wt.%, 0.30wt.% or 0.35wt.%, and the percentage refers to the RTB-based permanent magnet material The percentage of mass in the composition of raw materials.
- the content of Mn is preferably 0.0-0.03wt.%, but not 0, such as 0.01wt.%, and the percentage refers to the raw material composition of the RTB-based permanent magnet material The percentage of mass.
- the R-T-B-based permanent magnetic material may also include conventional additive elements M, such as one or more of Ni, Zn, Ag, In, Sn, Bi, V, Cr, Hf, Ta, and W.
- conventional additive elements M such as one or more of Ni, Zn, Ag, In, Sn, Bi, V, Cr, Hf, Ta, and W.
- the type of M is preferably Cr.
- the content of M is preferably 0-0.15wt.%, but not 0, such as 0.05wt.% or 0.12wt.%, and the percentage refers to the mass in the raw material composition of the RTB-based permanent magnet material percentage.
- the raw material composition of the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, Cu: 0.2-0.5wt. %, B: 0.95-1.1wt.%, Fe: 61.5-69.5wt.%, the percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the raw material composition of the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, Al: 0-0.8wt. %, but not 0, B: 0.95-1.1wt.%, Fe: 61.5-69.5wt.%, the percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the raw material composition of the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, Ga: 0.1-1.85wt. %, B: 0.95-1.1wt.%, Fe: 61.5-69.5wt.%, the percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the raw material composition of the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, Co: 0.0-3.0wt. %, but not 0, B: 0.95-1.1wt.%, Fe: 61.5-69.5wt.%, the percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the raw material composition of the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, Zr: 0.25-0.35wt. %, B: 0.95-1.1wt.%, Fe: 61.5-69.5wt.%, the percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the raw material composition of the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, Nb: 0.25-0.35wt. %, B: 0.95-1.1wt.%, Fe: 61.5-69.5wt.%, the percentage refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the raw material composition of the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, Cu: 0.34-0.5wt %, Al: 0-0.8wt.%, but not 0, B: 0.95-1.1wt.%, Fe: 61.5-69.5wt.%, the percentage refers to the raw material composition of the RTB-based permanent magnet material The mass percentage in.
- the raw material composition of the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, Cu: 0.34-0.5wt %, Al: 0-0.8wt.%, but not 0, Ga: 0.1-0.5wt.%, B: 0.95-1.1wt.%, Fe: 61.5-69.5wt.%, the percentages refer to the The mass percentage in the raw material composition of the RTB-based permanent magnet material.
- the raw material composition of the RTB-based permanent magnet material includes the following components: R': 29.5-33.5wt.%, Pr ⁇ 8.85wt.%, Cu: 0.34-0.5wt .%, Al: 0.3-0.8wt.%, Ga: 0.1-0.4wt.%, Zr: 0.25-0.30wt.%, B: 0.95-1.1wt.%, Fe: 61.5-69.5wt.%, the percentage is Refers to the mass percentage in the raw material composition of the RTB-based permanent magnet material.
- 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 melting furnace may be 5 ⁇ 10 -2 Pa.
- the temperature of the smelting may be 1500°C or less.
- the casting process can be a conventional casting process in the field, for example: in an Ar atmosphere (for example, under an Ar atmosphere of 5.5 ⁇ 10 4 Pa), the temperature of 10 2 °C/sec-10 4 °C/sec Speed cooling is enough.
- the hydrogen breaking process can be a conventional hydrogen breaking 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 conditions 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 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.
- the oxygen content O in the grinding atmosphere is 0-50 ppm, such as 0 ppm, 5 ppm, 10 ppm, 15 ppm, 20 ppm, 25 ppm, 30 ppm, 35 ppm, 40 ppm, 45 ppm or 50 ppm.
- the dispersant may be a dispersant conventionally added during the preparation process of the R-T-B series permanent magnetic material, and is generally a lubricant and/or an antioxidant.
- the lubricant and antioxidant added in the preparation process of the R-T-B permanent magnet material contain C element.
- the lubricant may be zinc stearate.
- the content of the dispersant is preferably 0.04-0.14%, such as 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, 0.11%, 0.12%, 0.13% or 0.14% , Percentage refers to the mass percentage of the total mass of the powder after mixing.
- the amount of zinc stearate can be 0.04-0.14%, such as 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, 0.11%, 0.12%, 0.13% or 0.14%, the percentage refers to the mass percentage of the total mass of the powder after mixing.
- the oxygen content O in the pressing atmosphere is 10-30 ppm, such as 10 ppm, 12 ppm, 14 ppm, 16 ppm, 18 ppm, 20 ppm, 22 ppm, 24 ppm, 26 ppm, 28 ppm or 30 ppm.
- 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 a preheating at a temperature of 300°C and 600°C for 1 hour each.
- the sintering temperature may be a conventional sintering temperature in the art, for example, 1040-1090°C, and for example, 1050°C.
- the sintering time may be a conventional sintering time in the field, for example, 2h.
- Ar can be passed through before the cooling to make the air pressure reach 0.1 MPa.
- a grain boundary diffusion treatment is further performed.
- the grain boundary diffusion treatment can be processed according to a conventional process in the art, for example, the surface of the RTB-based permanent magnet material is vapor-deposited, coated or sputtered to attach a substance containing Tb and/or a substance containing Dy , After diffusion heat treatment, it is enough.
- the Tb-containing substance may be Tb metal, Tb-containing compound (for example, Tb-containing fluoride) or alloy.
- the Dy-containing substance may be Dy metal, Dy-containing compound (for example, Dy-containing fluoride) or alloy.
- the temperature of the diffusion heat treatment may be 800-900°C, for example 850°C.
- the time of the diffusion heat treatment may be 12-48h, such as 24h.
- the treatment temperature of the aging treatment is preferably 500-650°C, such as 600-650°C, and further for example 630°C.
- the heating rate to 500-650°C is preferably 3-5°C/min.
- the starting point of the temperature increase may be room temperature.
- the treatment time of the aging treatment 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.
- the application fields can be the automotive drive field, the wind power field, the servo motor and the home appliance field (for example, air conditioner).
- the room temperature refers to 25°C ⁇ 5°C.
- Pr is praseodymium
- Nd is neodymium
- Cu is copper
- B boron
- Fe is iron
- Al aluminum
- Ga gallium
- Co cobalt
- Zr zirconium
- Ti titanium
- Nb niobium
- Zn Zinc
- Dy is dysprosium
- Tb is terbium
- Mn manganese
- Ni nickel
- Ag silver
- In indium
- Sn is tin
- Bi bismuth
- V vanadium
- Cr is chromium
- Ta tantalum
- W is tungsten
- O oxygen
- C carbon
- N nitrogen.
- the reagents and raw materials used in the present invention are all commercially available.
- the RTB-based permanent magnetic material in the present invention can realize the improvement of the performance of the permanent magnetic material without heavy rare earths.
- the RTB-based permanent magnetic material has excellent magnetic properties, high coercivity, high remanence and temperature stability. it is good.
- Fig. 1 is a scanning photograph of the microstructure of the R-T-B permanent magnetic material prepared in Example 68, in which the position indicated by a is the intercrystalline triangle region.
- wt.% refers to the mass percentage of the components in the raw material composition of the R-T-B permanent magnetic material, and "/" means that the element is not added.
- Br is the remanence
- Hcj is the intrinsic coercivity.
- 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 pass 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 to fully dehydrogenate; then cooling is performed to take out the powder after hydrogen breakage and pulverization.
- Fine pulverization process under a nitrogen atmosphere and the pressure of the pulverizing chamber is 0.38 MPa, the powder after hydrogen pulverization is subjected to jet mill pulverization for 3 hours to obtain a fine powder.
- the oxygen content (ppm) in the nitrogen atmosphere is shown in Table 2.
- Magnetic field forming process using a right-angle orientation 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 molding.
- the O (oxygen) content in the atmosphere during the pressing process is shown in Table 2.
- a secondary molding machine isostatic press
- each formed body is moved to a sintering furnace for sintering, sintered under a vacuum of 5 ⁇ 10 -3 Pa and maintained at a temperature of 300°C and 600°C for 1 hour; then, heat at 1050°C The temperature is sintered for 2 hours; then Ar is introduced to make the air pressure reach 0.1 MPa, and then cooled to room temperature.
- Example 2 The formulations of Example 2 to Example 75 and Comparative Example 1-2 are shown in Table 1, and the preparation process is shown in Table 2, and the rest of the steps are the same as in Example 1.
- Example 2 The sintered body obtained in Example 1 was first subjected to grain boundary diffusion treatment, and then subjected to aging treatment.
- the preparation process is shown in Table 2, and the other steps are the same as in Example 1.
- the grain boundary diffusion treatment process is as follows:
- the sintered body is processed into a magnet with a diameter of 20mm and a sheet thickness of less than 7mm.
- the thickness direction is the direction of the magnetic field orientation.
- raw materials prepared with Dy fluoride are used to spray and coat the magnet on the entire surface.
- the magnet is dried, in a high-purity Ar atmosphere, the metal with Dy element is sputtered on the surface of the magnet, and the diffusion heat treatment is performed at a temperature of 850°C for 24 hours. Cool to room temperature.
- Example 2 The sintered body obtained in Example 1 was first subjected to grain boundary diffusion treatment, and then subjected to aging treatment.
- the preparation process is shown in Table 2, and the other steps are the same as in Example 1.
- the grain boundary diffusion treatment process is as follows:
- the sintered body is processed into a magnet with a diameter of 20mm and a sheet thickness of less than 7mm.
- the thickness direction is the direction of the magnetic field orientation.
- the raw materials made of Tb fluoride are used to spray and coat the magnet on the entire surface.
- the magnet is dried, and in a high-purity Ar atmosphere, the metal with Tb element is sputtered on the surface of the magnet, and the diffusion heat treatment is performed at 850°C for 24 hours. Cool to room temperature.
- the percentage of zinc stearate added refers to the weight percentage of the mixed powder, and the O (oxygen) content refers to the content of O (oxygen) atoms in the atmosphere.
- Magnetic performance evaluation The permanent magnet material uses the NIM-10000H BH bulk rare earth permanent magnet non-destructive measurement system of China Metrology Institute for magnetic performance testing. Table 3 below shows the magnetic performance test results.
- each component was measured using a high-frequency inductively coupled plasma emission spectrometer (ICP-OES. Table 4 below shows the component detection results.
- FE-EPMA test compare the example numbers in Table 4 as 1, 2, 11, 12, 21, 23, 34, 35, 39, 43, 51, 52, 60, 63, 68, 69 and comparative examples
- the vertical orientation surfaces of the RTB-based magnet materials of 1 and Comparative Example 2 were polished and tested with a field emission electron probe microanalyzer (FE-EPMA) (JEOL, 8530F).
- FE-EPMA field emission electron probe microanalyzer
- Example 68 The position of the intergranular triangular region in Example 68 (as shown in position a in Figure 1) was tested for composition and the phase of the triangular region (rare-earth-rich phase) and all phases of the observation surface (main phase, grain boundary phase and rich phase) were determined.
- the relative volume ratio of the rare earth phase it can be found that in the samples containing high Pr and high C, the phase ratio formed by the intergranular triangle region is relatively low, but there is no such phenomenon in the samples with low Pr.
- Table 5 The specific test results are shown in Table 5 below.
- the mass ratio of R', Ga, Cu and O in the intercrystalline triangle region refers to the mass percentage of the total mass of the elements in the intercrystalline triangle region;
- the volume ratio of the intercrystalline triangle region phase refers to the intercrystalline triangle region phase The percentage of the total volume of the "main phase, grain boundary phase and intergranular triangle area”.
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Abstract
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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’:29.5-33.5wt.%;其中:所述R’为稀土元素,所述R’包括Pr,所述Pr的含量≥8.85wt.%;C:0.106-0.26wt.%;O:≤0.07wt.%;X:0-5.0wt.%,所述X为Cu、Al、Ga、Co、Zr、Ti、Nb和Mn中的一种或多种;B:0.90-1.2wt.%;Fe:61.4-69.5wt.%。
- 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29.5-33.4wt.%,例如29.5wt.%、30.5wt.%、30.8wt.%、31.0wt.%、31.013wt.%、31.075wt.%、31.115wt.%、31.5wt.%、32.0wt.%、32.3wt.%、32.8wt.%或33.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述Pr的含量为8.85-27.15wt.%,优选为≥17.00wt.%,例如8.846wt.%、8.848wt.%、8.849wt.%、8.851wt.%、9.852wt.%、10.148wt.%、10.151wt.%、10.848wt.%、10.849wt.%、11.848wt.%、12.148wt.%、12.15wt.%、12.151wt.%、13.149wt.%、14.147wt.%、14.148wt.%、14.149wt.%、14.151wt.%、14.152wt.%、16.148wt.%、16.151wt.%、16.152wt.%、17.148wt.%、17.149wt.%、17.15wt.%、17.151wt.%、17.152wt.%、18.148wt.%、18.149wt.%、18.151wt.%、18.152wt.%、19.148wt.%、19.149wt.%、19.15wt.%、19.151wt.%、19.152wt.%、20.148wt.%、20.149wt.%、20.15wt.%、20.152wt.%、21.148wt.%、22.149wt.%、22.151wt.%、23.149wt.%、23.15wt.%、24.148wt.%、24.151wt.%、24.152wt.%、25.152wt.%或27.148wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述R’中还包括Nd和/或R,所述R为除Pr、Nd外的稀土元素;其中:所述Nd的含量优选为3.3-23.0wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;所述Nd和所述R’的质量比优选为≤0.72,更优选为<0.5;所述R的种类优选为Y和/或Ce;所述R的含量优选为0-1wt.%,例如0.29wt.%,百分比是指在所述R-T-B系永磁材料中质量百分比;和/或,所述R’中还包括重稀土元素RH;其中:所述RH的种类优选为Dy和/或Tb;所述RH的含量优选为0.5-2.6wt.%,例如0.58wt.%、0.62wt.%、1.212wt.%、1.219wt.%、1.51wt.%、1.991wt.%、2.011wt.%、2.511wt.%或2.512wt.%,百分比是指在所述R-T-B系永磁材料中质量百分比;所述RH和所述R的质量比优选为<0.253,例如0.019-0.075;当所述RH中含有Tb时,所述Tb的含量优选为0.5-2.0wt.%,例如1.991wt.%、1.212wt.%、 1.219wt.%或0.58wt.%,百分比是指在所述R-T-B系永磁材料中质量百分比;当所述RH中含有Dy时,所述Dy的含量优选为0.6-2.52wt.%,例如0.62wt.%、1.51wt.%、2.011wt.%、2.511wt.%或2.512wt.%,百分比是指在所述R-T-B系永磁材料中质量百分比;和/或,所述C的含量为0.106-0.25wt.%,例如0.1062wt.%、0.1069wt.%、0.1072wt.%、0.1075wt.%、0.1251wt.%、0.1253wt.%、0.1256wt.%、0.1532wt.%、0.1534wt.%、0.1537wt.%、0.1759wt.%、0.1761wt.%、0.1764wt.%、0.1835wt.%、0.184wt.%、0.1843wt.%、0.1846wt.%、0.1965wt.%、0.197wt.%、0.1973wt.%、0.2139wt.%、0.2144wt.%、0.2147wt.%、0.2243wt.%、0.2245wt.%、0.2248wt.%、0.2251wt.%、0.2379wt.%或0.2456wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述O的含量为≤0.0691wt.%,例如0.0382wt.%、0.0384wt.%、0.039wt.%、0.0391wt.%、0.041wt.%、0.0412wt.%、0.0432wt.%、0.0442wt.%、0.0444wt.%、0.0456wt.%、0.0458wt.%、0.0468wt.%、0.0492wt.%、0.0493wt.%、0.0494wt.%、0.05wt.%、0.0501wt.%、0.0503wt.%、0.0523wt.%、0.0529wt.%、0.0531wt.%、0.0558wt.%、0.0564wt.%、0.0566wt.%、0.0582wt.%、0.0588wt.%、0.059wt.%、0.0635wt.%、0.0641wt.%、0.0643wt.%、0.0669wt.%、0.0675wt.%、0.0685wt.%或0.0691wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述B的含量为0.94-1.1wt.%,例如0.946wt.%、0.947wt.%、0.948wt.%、0.949wt.%、0.951wt.%、0.952wt.%、0.958wt.%、0.961wt.%、0.962wt.%、0.981wt.%、0.982wt.%、0.985wt.%、0.998wt.%、1.008wt.%、1.009wt.%、1.01wt.%、1.011wt.%或1.012wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述Fe的含量为61.4-69.3wt.%,例如61.49wt.%、61.60wt.%、62.15wt.%、62.19wt.%、62.66wt.%、62.91wt.%、63.52wt.%、63.62wt.%、63.66wt.%、64.71wt.%、65.85wt.%、66.02wt.%、66.15wt.%、66.19wt.%、66.22wt.%、66.23wt.%、66.30wt.%、66.37wt.%、66.40wt.%、66.44wt.%、66.57wt.%、66.66wt.%、66.70wt.%、66.72wt.%、66.75wt.%、66.82wt.%、66.85wt.%、66.88wt.%、66.91wt.%、66.94wt.%、66.95wt.%、66.98wt.%、67.08wt.%、67.15wt.%、67.17wt.%、67.23wt.%、67.27wt.%、67.29wt.%、67.30wt.%、67.31wt.%、67.32wt.%、67.34wt.%、67.40wt.%、67.42wt.%、67.47wt.%、67.48wt.%、67.54wt.%、67.64wt.%、67.65wt.%、67.69wt.%、67.71wt.%、67.74wt.%、67.78wt.%、67.80wt.%、68.22wt.%、68.24wt.%、68.25wt.%、68.27wt.%、68.28wt.%、68.31wt.%、68.32wt.%、68.34wt.%、68.36wt.%、68.73wt.%、68.83wt.%、68.95wt.%、69.03wt.%、69.10wt.%或69.25wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述R-T-B系永磁材料中还包括M,所述M为Ni、Zn、Ag、In、Sn、Bi、V、Cr、Hf、Ta和W中的一种或多种;其中:所述M的种类优选为Cr;所述M的含量优选为0-0.15wt.%、但不为0,例如0.05wt.%或0.12wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述R-T-B系永磁材料中还包含氮元素N,优选地,所述N元素的含量≤0.05wt.%,例如0.0182wt.%、0.0187wt.%、0.0223wt.%、0.0228wt.%、0.025wt.%、0.0251wt.%、0.0256wt.%、0.0284wt.%、0.0285wt.%、0.029wt.%、0.0301wt.%、0.0302wt.%、0.0307wt.%、0.0341wt.%、0.0342wt.%、0.0347wt.%、0.0366wt.%、0.0371wt.%、0.0372wt.%、0.0375wt.%、0.0378wt.%、0.0397wt.%、0.0398wt.%、0.0401wt.%、0.0404wt.%、0.0436wt.%、0.0439wt.%、0.0442wt.%、0.0455wt.%、0.0458wt.%、0.0461wt.%、0.0476wt.%、0.0482wt.%、0.0485wt.%或0.0486wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;和/或,所述R-T-B系永磁材料中包括主相、晶界相和晶间三角区,所述晶间三角区的体积占“所述主相、所述晶界相和所述晶间三角区”体积之和的百分比≤9.0%,例如3.2%、3.3%、3.7%、4.6%、4.8%或5.3%。
- 如权利要求1所述的R-T-B系永磁材料,其特征在于,所述X为Cu、Al、Ga、Co、Zr、Ti或Nb,或者,“Cu和Al”、“Ga和Mn”、“Cu、Al和Ga”、“Cu、Al、Ga和Zr”、“Cu、Al、Ga和Co”或“Cu、Al、Ga、Zr和Co”;和/或,所述X的含量优选为0-4.5wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;当所述X中包含Cu时,所述Cu的含量优选为0.2-0.51wt.%,例如0.201wt.%、0.302wt.%、0.34wt.%、0.341wt.%、0.351wt.%、0.381wt.%、0.382wt.%、0.4wt.%、0.401wt.%、0.402wt.%、0.403wt.%、0.41wt.%、0.42wt.%、0.421wt.%、0.441wt.%、0.451wt.%、0.5wt.%、0.501wt.%或0.502wt.%,百分比是指在所述R-T-B系永磁材料中质量百分比;当所述X中包含Al时,所述Al的含量优选为0-0.81wt.%、但不为0,例如0.01-0.03wt.%或0.5-0.8wt.%,再例如0.01wt.%、0.021wt.%、0.03wt.%、0.041wt.%、0.042wt.%、0.101wt.%、0.102wt.%、0.103wt.%、0.202wt.%、0.298wt.%、0.301wt.%、0.302wt.%、0.351wt.%、0.401wt.%、0.402wt.%、0.403wt.%、0.451wt.%、0.497wt.%、0.501wt.%、0.502wt.%、0.601wt.%、0.602wt.%、0.702wt.%、0.801wt.%、0.802wt.%或0.81wt.%,百分比是指在所述R-T-B系永磁材料中质量百分比;当所述X中包含Ga时,所述Ga的含量优选为0.0-1.85wt.%、但不为0,更优选为0.1-1.552wt.%,例如0.102wt.%、0.151wt.%、0.202wt.%、0.251wt.%、0.3wt.%、0.301wt.%、0.302wt.%、0.399wt.%、0.401wt.%、0.42wt.%、0.421wt.%、0.501wt.%、0.502wt.%、0.901wt.%、1.402wt.%或1.552wt.%,百分比是指在所述R-T-B系永磁材料中质量百分比;当所述X中包含Co时,所述Co的含量优选为0.0-3.0wt.%、但不为0,更优选为0.5-2.5wt.%,例如0.5wt.%、1.0wt.%或2.5wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;当所述X中包含Zr时,所述Zr的含量优选为0.25-0.35wt.%,例如0.25wt.%、0.30wt.%或0.35wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;当所述X中包含Nb时,所述Nb的含量优选为0.25-0.35wt.%,例如0.25wt.%、0.30wt.%或0.35wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;当所述X中包含Mn时,所述Mn的含量优选为0.0-0.03wt.%、但不为0,例如0.01wt.%,百分比是指在所述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系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Cu:0.2-0.51wt.%,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Al:0-0.81wt.%、但不为0,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Ga:0.1-1.85wt.%,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Co:0.0-3.0wt.%、但不为0,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Zr:0.25-0.35wt.%,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Nb:0.25-0.35wt.%,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C: 0.106-0.25wt.%,O:≤0.07wt.%,Cu:0.34-0.51wt.%,Al:0-0.81wt.%、但不为0,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Cu:0.34-0.51wt.%,Al:0-0.81wt.%、但不为0,Ga:0.1-0.5wt.%,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Cu:0.34-0.51wt.%,Al:0.25-0.81wt.%,Ga:0.1-0.42wt.%,Zr:0.25-0.30wt.%,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Cu:0.34-0.51wt.%,Al:0.25-0.81wt.%,Ga:0.1-0.41wt.%,Co:0.0-3.0wt.%,Zr:0.25-0.30wt.%,Cr:0.05-0.12wt.%,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,RH:0.5-2.6wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Cu:0.34-0.51wt.%,Al:0.25-0.81wt.%,Ga:0.1-0.41wt.%,Co:0.0-3.0wt.%,Zr:0.25-0.30wt.%,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比;或者,所述R-T-B系永磁材料包括下述组分:R’:29.5-33.5wt.%,Pr≥8.85wt.%,Ce:0-1wt.%,RH:0.5-2.6wt.%,C:0.106-0.25wt.%,O:≤0.07wt.%,Cu:0.34-0.51wt.%,Al:0.25-0.81wt.%,Ga:0.1-0.41wt.%,Co:0.0-3.0wt.%,Zr:0.25-0.30wt.%,B:0.94-1.1wt.%,Fe:61.4-69.3wt.%,百分比是指在所述R-T-B系永磁材料中的质量百分比。
- 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:将所述R-T-B系永磁材料的原料组合物的熔融液经铸造、氢破、粉碎得粉体,将所述粉体和分散剂混合,再经压制、成形、烧结和时效处理,即可;其中:(1)所述R-T-B系永磁材料的原料组合物中,以质量百分比计,其包括下述组分:R’:29.5-33.5wt.%;所述R’为稀土元素,所述R’包括Pr,所述Pr的含量≥8.85wt.%;X:0-5.0wt.%,所述X为Cu、Al、Ga、Co、Zr、Ti、Nb和Mn中的一种或多种;B:0.90-1.2wt.%;Fe:61.4-69.5wt.%;(2)所述粉碎过程中,粉碎气氛中O≤60ppm;(3)所述压制过程中,压制气氛中O≤40ppm;(4)所述分散剂中含有C元素,且所述分散剂在混合后粉末中的质量百分比为0.04-0.2%。
- 如权利要求5所述的R-T-B系永磁材料的制备方法,其特征在于,所述R’的含量为29.5-33.3wt.%,优选为29.5wt.%、30.5wt.%、30.8wt.%、31wt.%、31.5wt.%、32wt.%、32.3wt.%、32.8wt.%或33.3wt.%,百分比是指在所述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Pr的含量为8.85-27.15wt.%,例如8.85wt.%、9.85wt.%、10.15wt.%、10.85wt.%、11.85wt.%、12.15wt.%、13.15wt.%、14.15wt.%、16.15wt.%、17.15wt.%、18.15wt.%、19.15wt.%、20.15wt.%、21.15wt.%、22.15wt.%、23.15wt.%、24.15wt.%、25.15wt.%或27.15wt.%,百分比是指在所述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R’中还包括Nd和/或R,所述R为除Pr、Nd外的稀土元素;其中,所述Nd的含量优选为3.35-22.65wt.%,更优选为3.35wt.%、5.35wt.%、6.65wt.%、6.85wt.%、7.35wt.%、7.85wt.%、8.35wt.%、8.65wt.%、8.85wt.%、9.35wt.%、10.65wt.%、10.85wt.%、11.35wt.%、11.65wt.%、11.85wt.%、12.35wt.%、12.65wt.%、13.35wt.%、13.65wt.%、13.85wt.%、14.35wt.%、14.65wt.%、14.85wt.%、15.35wt.%、16.35wt.%、16.65wt.%、16.85wt.%、17.35wt.%、17.65wt.%、18.35wt.%、18.65wt.%、18.85wt.%、19.35wt.%、19.65wt.%、20.65wt.%、20.85wt.%、21.35wt.%、21.65wt.%、21.95wt.%、22.15wt.%或22.65wt.%,百分比是指在所述R-T-B系永磁材料的原料组合物中的质量百分比;所述Nd和所述R’的质量比优选为≤0.72;所述R的种类优选为Y和/或Ce;所述R的含量优选为0-1wt.%,例如0.3wt.%,百分比是指在所述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R’中还包括重稀土元素RH;所述RH的种类优选为Dy和/或Tb;所述RH的含量优选为1.2-2.5wt.%,例如1.2wt.%、1.5wt.%、2wt.%或2.5wt.%,百分比是指在所述R-T-B系永磁材料的原料组合物中的质量百分比;所述RH和所述R’的质量比优选为<0.253,例如0.038-0.075,再例如0.038、0.039、0.046、0.061或0.075;当所述RH中含有Tb时,所述Tb的含量优选为1.2-2.0wt.%,例如1.2wt.%或2.0wt.%,百分比是指在所述R-T-B系永磁材料的原料组合物中的质量百分比;当所述RH中含有Dy时,所述Dy的含量优选为1.5-2.5wt.%,例如1.5wt.%、2.0wt.%或2.5wt.%,百分比是指在所述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0.95-1.1wt.%,例如0.95wt.%、0.96wt.%、0.98wt.%或1.01wt.%,百分比是指在所述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Fe的含量为61.5-69.5wt.%,例如61.79wt.%、61.89wt.%、62.44wt.%、62.89wt.%、63.24wt.%、63.84wt.%、63.87wt.%、63.94wt.%、64.99wt.%、66.19wt.%、66.29wt.%、66.47wt.%、66.52wt.%、66.55wt.%、66.61wt.%、66.69wt.%、66.75wt.%、66.85wt.%、66.97wt.%、67.00wt.%、67.02wt.%、67.068wt.%、67.13wt.%、67.14wt.%、67.19wt.%、67.24wt.%、67.25wt.%、67.35wt.%、67.37wt.%、67.45wt.%、67.49wt.%、67.54wt.%、67.55wt.%、67.57wt.%、67.59wt.%、67.64wt.%、67.65wt.%、67.69wt.%、67.718wt.%、67.75wt.%、67.85wt.%、67.95wt.%、67.96wt.%、67.97wt.%、68.008wt.%、68.12wt.%、68.55wt.%、68.62wt.%、69.02wt.%、69.1wt.%、69.22wt.%、69.27wt.%、69.32wt.%或69.45wt.%,百分比是指在所述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X为Cu、Al、Ga、Co、Zr、Ti或Nb,或者,“Cu和Al”、“Ga和Mn”、“Cu、Al和Ga”、“Cu、Al、Ga和Zr”、“Cu、Al、Ga和Co”或“Cu、Al、Ga、Zr和Co”;和/或,所述X的含量为0-4.5wt.%;当所述X中包含Cu时,所述Cu的含量优选为0.2-0.5wt.%;当所述X中包含Al时,所述Al的含量优选为0-0.8wt.%、但不为0,例如0.01-0.03wt.%或0.5-0.8wt.%;当所述X中包含Ga时,所述Ga的含量优选为0.0-1.85wt.%、但不为0,更优选为0.1-1.55wt.%;当所述X中包含Co时,所述Co的含量优选为0.0-3.0wt.%、但不为0,更优选为0.5-2.5wt.%;当所述X中包含Zr时,所述Zr的含量优选为0.25-0.35wt.%;当所述X中包含Nb时,所述Nb的含量优选为0.25-0.35wt.%;当所述X中包含Mn时,所述Mn的含量优选为0.0-0.03wt.%、但不为0;百分比是指在所述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R-T-B系永磁材料中还包括M,所述M为Ni、Zn、Ag、In、Sn、Bi、V、Cr、Hf、Ta和W中的一种或多种;其中,所述M的种类优选为Cr;所述M的含量优选为0-0.15wt.%、但不为0,百分比是指在所述R-T-B系永磁材料的原料组合物中的质量百分比。
- 如权利要求5或6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:在真空感应熔炼炉中熔炼,即可;所述熔炼炉的真空度可为5×10 -2Pa;所述熔炼的温度可为1500℃以下;和/或,所述铸造的工艺按下述步骤进行:在Ar气氛中,以10 2℃/秒-10 4℃/秒的速度冷却,即可;和/或,所述粉碎为气流磨粉碎;所述气流磨粉碎的粉碎室压力可为0.38MPa;所述气流磨粉碎的时间可为3小时;和/或,所述烧结之前还进行预热;其中,所述预热的温度可为300-600℃,所述预热的时间可为1-2h;优选地,所述预热为在300℃和600℃的温度下各预热1h;和/或,所述烧结的温度为1040-1090℃;和/或,所述烧结的时间为2h;和/或,所述烧结之后、所述时效处理之前,还进行晶界扩散处理;其中,优选地,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的物质和/或含有Dy的物质,经扩散热处理,即可;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,所述时效处理的处理温度为500-650℃;和/或,所述时效处理中,升温至500-650℃的升温速率为3-5℃/min;和/或,所述时效处理的处理时间为3h。
- 如权利要求5或6所述的R-T-B系永磁材料的制备方法,其特征在于,所述粉碎过程中,粉碎气氛中氧含量O为0-50ppm,例如0ppm、5ppm、10ppm、15ppm、20ppm、25ppm、30ppm、35ppm、40ppm、45ppm或50ppm;和/或,所述分散剂为润滑剂和/或抗氧化剂,所述润滑剂优选为硬脂酸锌;当所述分散剂中包含硬脂酸锌时,所述硬脂酸锌的用量可为0.04-0.14%,例如0.04%、0.05%、0.06%、0.07%、0.08%、0.09%、0.1%、0.11%、0.12%、0.13%或0.14%,百分比是指占混合后粉末总质量的质量百分比;和/或,所述分散剂的含量为0.04-0.14%,例如0.04%、0.05%、0.06%、0.07%、0.08%、0.09%、0.1%、0.11%、0.12%、0.13%或0.14%,百分比是指占混合后粉末总质量的质量百分比;和/或,所述压制过程中,压制气氛中氧含量O为10-30ppm,例如10ppm、12ppm、14ppm、16ppm、18ppm、20ppm、22ppm、24ppm、26ppm、28ppm或30ppm。
- 一种如权利要求5-8中任一项所述的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和9中任一项所述的R-T-B系永磁材料作为电子元器件的应用。
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TWI751843B (zh) | 2022-01-01 |
TW202125544A (zh) | 2021-07-01 |
EP3940724A1 (en) | 2022-01-19 |
JP7253071B2 (ja) | 2023-04-05 |
KR20210151946A (ko) | 2021-12-14 |
CN110942878B (zh) | 2021-03-26 |
CN110942878A (zh) | 2020-03-31 |
EP3940724A4 (en) | 2022-07-13 |
KR102527122B1 (ko) | 2023-04-27 |
JP2022535482A (ja) | 2022-08-09 |
US20220328220A1 (en) | 2022-10-13 |
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