Preparation method of improved sintered neodymium-iron-boron (Nd—Fe—B) casting strip

Abstract

A preparation method of improved sintered neodymium-iron-boron (Nd—Fe—B) casting strips includes the following steps: firstly nucleation assisted alloy particles used for sintered Nd—Fe—B casting strips are prepared, all elements are weighted as follows: 26.68-28% of Pr—Nd, 70-72.5% of Fe and 0.90-1% of B, and a Pr element in two elements of Pr—Nd accounts for 0-30 wt %; the compounded materials are smelted and poured to obtain alloy strips, then the alloy strips are crushed into particles with diameter of 1-10 mm; secondly, Nd—Fe—B casting strips are prepared: the prepared intermediate materials are smelted and melted into molten steel, and then are refined; after the intermediate materials are fully melted, the nucleation assisted alloy particles are added; and after the nucleation assisted alloy particles are added, smelting is performed for 3-15 minutes pouring is performed, and final Nd—Fe—B alloy casting strips are obtained.

Claims

1. A method for preparing a sintered Nd—Fe—B casting strip, the method comprising the following steps: 1) preparing nucleation assisted alloy particles used for the sintered Nd—Fe—B casting strip; 1.1) weighing the following nucleation assisted alloy particle elements: 26.68-28 wt % of Pr—Nd, 70-72.5% of Fe and 0.90-1% of B, wherein a Pr element in two elements of Pr—Nd accounts for 0-30 wt %, and obtaining an alloy strip with a proportion of ingredient atoms close to that of (Pr—Nd).sub.2Fe.sub.14B through conventional compounding, smelting and pouring; and 1.2) crushing the alloy strip into particles with a diameter in the range from 1-10 mm, to serve as the nucleation assisted alloy particles used for the sintered Nd—Fe—B casting strip; 2) preparing the sintered Nd—Fe—B casting strip; 2.1) providing an intermediate material, wherein composition of the intermediate material is calculated according to the composition of the Nd—Fe—B casting strip to be prepared and an additional quantity of the nucleation assisted alloy particles, and the additional quantity of the nucleation assisted alloy particles is in the range from 3-6% by weight, based on a total weight of the sintered Nd—Fe—B casting strip; and 2.2) melting the intermediate material and smelting for 10-20 minutes to obtain a smelted intermediate material, adding the nucleation assisted alloy particles into the smelted intermediate material, further smelting for 3-15 minutes under a condition that power is reduced by 150-250 KW from a power for smelting the intermediate material, and pouring, thereby obtaining the sintered Nd—Fe—B alloy casting strip.

2. The method as claimed in claim 1, wherein the step of crushing further comprises mechanical crushing or hydrogen crushing.

3. The method as claimed in claim 2, wherein the step of crushing comprises hydrogen crushing, and hydrogen crushing further comprises dehydrogenation and hydrogen content in the nucleation assisted alloy particles is smaller than 1000 ppm.

4. The method as claimed in claim 1, wherein the additional quantity of the nucleation assisted alloy particles is 5% by weight, based on a total weight of the sintered Nd—Fe—B casting strip.

5. The method as claimed in claim 2, wherein the additional quantity of the nucleation assisted alloy particles is 5% by weight, based on a total weight of the sintered Nd—Fe—B casting strip.

6. The method as claimed in claim 3, wherein the additional quantity of the nucleation assisted alloy particles is 5% by weight, based on a total weight of the sintered Nd—Fe—B casting strip.

7. The method as claimed in claim 1, wherein in the step 1.1, an Fe element in the nucleation assisted alloy particles is replaced with a Co element, and the Co element accounts for 0-5 wt % of the nucleation assisted alloy particles.

8. The method as claimed in claim 2, wherein, in the step 1.1, an Fe element in the nucleation assisted alloy particles is replaced with a Co element, and the Co element accounts for 0-5 wt % of the nucleation assisted alloy particles.

9. The method as claimed in claim 3, wherein in step 1.1, an Fe element in the nucleation assisted alloy particles is replaced with a Co element, and the Co element accounts for 0-5 wt % of the nucleation assisted alloy particles.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIGS. 1A and 1B show a comparison of metallographic phases of casting strips obtained by a technique disclosed by the present disclosure and those by a traditional technology: FIG. 1A shows an image of the metallographic phases by a nucleation assisted technique. FIG. 1B shows an image of the metallographic phases by the traditional technology; and

(2) FIGS. 2A and 2B show a comparison of the metallographic phases of the casting strips obtained by the nucleation assisted technique and those by the traditional technology: FIG. 2A shows an image of the metallographic phases by a nucleation assisted technique. FIG. 2B shows an image of the metallographic phases by the traditional technology.

DETAILED DESCRIPTION OF THE EMBODIMENTS

(3) To enable those skilled in the art to better understand the technical solution of the present disclosure, the present disclosure will be described in detail below with reference to the accompanying drawings. The description in this section is merely exemplary and explanatory and should not have any limitation on the scope of protection of the present disclosure.

Example 1

(4) 1) A formula of nucleation assisted alloys (A material) in the example was designed as: Pr—Nd.sub.28Fe.sub.69.5Co.sub.1.5B.sub.1, with an added weight percent of 5%, where the ingredients of the alloys were calculated before addition of the nucleation assisted alloys according to the design, and ingredients of the intermediate materials were obtained as follows:

(5) Pr—Nd.sub.25.9Dy.sub.4.42Fe.sub.balCo.sub.1.5B.sub.0.98M.sub.0.96 (M=Al, Cu, Nb, Ga), where M was an impurity element, and bal represented balance; and

(6) the intermediate materials accounted for 95% in the final Nd—Fe—B casting strips (C materials). The final formula of the Nd—Fe—B casting strips (C materials) was designed as (in a weight percent): Pr—Nd.sub.26Dy.sub.4.2Fe.sub.balCo.sub.1.58B.sub.0.98M.sub.0.90 (M=Al, Cu, Nb, Ga).

(7) 2) The nucleation assisted alloys (A materials) were smelted. The compounded A materials were added into a smelting crucible, vacuumizing was performed until the intensity of pressure was smaller than or equal to 0.5 Pa, and the materials were heated and baked at a low power for 20 minutes. The materials were heated and baked at the largest power of 580 KW until furnace materials were melted through visual observation. Smelting was performed for 12 minutes under the condition that the power was reduced by 100 KW. The molten steel was poured out when the temperature of the molten steel was in the range of 1430-1450° C. During pouring, the rotating speed of a copper roller wheel of a smelting furnace was about 30-35 r/min. The linear speed of a corresponding molten steel swinging position was 0.96-1.12 m/s, and casting strips with thickness of 0.25-1 millimeter were obtained.

(8) The casting strips were crushed into particles with particle size diameter of about 1-10 mm by a mechanical crushing method as the nucleation assisted alloy particles.

(9) 3) The Nd—Fe—B casting strips (C material) were smelted. 570 Kg of the compounded intermediate materials were added into the smelting crucible, vacuumizing was performed until the intensity of pressure was smaller than or equal to 0.5 Pa, and the materials were heated and baked at a low power for 20 minutes. The materials were heated and baked at the largest power of 580 KW until the furnace materials were melted. Smelting was performed for 20 minutes after the smelting power was slightly regulated down to 480 KW. The nucleation assisted alloys, namely the materials A, were added through a special tool for later-added materials, arranged at a top end, and after the materials A were added, smelting was performed for 15 minutes after the power was regulated down to 300 KW, so that the nucleation assisted alloys, namely the materials A, in the molten steel were softened but not in a free atom state completely. The molten steel was poured out when the temperature was in the range of 1390-1400° C. During pouring, the rotating speed of the copper roller wheel of the smelting furnace was about 40-45 r/min, the linear speed of the corresponding molten steel swinging position was 1.28-1.44 m/s, and casting strips with thicknesses of 0.15-0.35 millimeter were obtained.

(10) Finally, with the same ingredients, comparison of metallographic phases of casting strips obtained by a technique disclosed by the present disclosure and those by a traditional technology was obtained. FIG. 1A shows an image of the metallographic phases by a nucleation assisted technique, and FIG. 1B shows an image of the metallographic phases by the traditional technology.

(11) The Nd—Fe—B casting strips were then subjected to conventional crushing and powdering, pressing and forming, and sintering so that the Nd—Fe—B finished products were obtained. A comparison table of properties of Nd—Fe—B finished products obtained by different technologies with the same ingredients is shown in the following Table 1. 1-1 # to 1-3 # show the properties of Nd—Fe—B magnets obtained by adopting the technique disclosed by the present disclosure, and 1-4 # to 1-6 # show the properties of Nd—Fe—B magnets obtained by adopting the traditional technology.

(12) TABLE-US-00001 TABLE 1 Comparison table of properties of Nd—Fe—B finished products obtained by different technologies with the same ingredients. (BH)max SN Br(T) Hcj(kAm/s) Hcb(kAm/s) (KJ/m3) Hk/Hcj 1-1# 1.251 2187 976 304 0.983 1-2# 1.253 2184 976 305 0.982 1-3# 1.249 2188 974 303 0.984 1-4# 1.268 2063 992 313 0.958 1-5# 1.267 2048 991 313 0.956 1-6# 1.268 2070 994 314 0.958

(13) It can be seen from FIGS. 1A and 1B and Table 1, after the technology and the technique were adopted, the metallographic phase quality of the casting strips was improved, the intrinsic coercivity Hcj of magnet finished products was improved, and residual magnetism was slightly reduced.

Example 2

(14) A formula of the nucleation assisted alloys (A materials) in the example was designed as Pr—Nd.sub.28Fe.sub.69.09Co.sub.2B.sub.0.91, with an added weight percent of 5%, where the ingredients of the alloys were calculated before addition of the nucleation assisted alloys according to the design, and ingredients of the intermediate materials were obtained as follows:

(15) Pr—Nd.sub.29.47Tb.sub.1.05Fe.sub.balCo.sub.2.0B.sub.0.93M.sub.0.59 (M=Al, Cu, Zr, Ga), and the intermediate materials accounted for 95 wt % in final (C materials).

(16) The final formula of the C materials was designed as (in a weight percent): Pr—Nd.sub.29.4Tb.sub.1Fe.sub.balCo.sub.2.0B.sub.0.93M.sub.0.55 (M=Al, Cu, Nb, Ga).

(17) 2) The nucleation assisted alloys (A materials) were smelted. The compounded A materials were added into the smelting crucible, vacuumizing was performed until the intensity of pressure was smaller than or equal to 0.5 Pa, and the materials were heated and baked at a low power for 20 minutes. The materials were heated and baked at the largest power of 580 KW until furnace materials were melted through visual observation. Smelting was performed for 5-10 minutes under the condition that the power was reduced by 20-50 KW. The molten steel was poured out when the temperature of the molten steel was in the range of 1450-1480° C. During pouring, the rotating speed of a copper roller wheel of a smelting furnace was about 30-35 r/min, the linear speed of a corresponding molten steel swinging position was 0.96-1.12 m/s, and casting strips with thicknesses of 0.25-1 mm were obtained.

(18) The casting strips were crushed into particles with particle size of about 1-10 mm by the mechanical crushing method, to be used as the nucleation assisted alloys.

(19) 3) The Nd—Fe—B casting strips (C materials) were smelted. 570 Kg of the compounded intermediate materials were added into the smelting crucible, vacuumizing was performed until the intensity of pressure was smaller than or equal to 0.5 Pa, and the materials were heated and baked at a low power for 20 minutes. The materials were heated at the largest power of 580 KW until the furnace materials were melted. Smelting was performed for 10-12 minutes after the smelting power was slightly regulated down to 450 KW. The nucleation assisted alloys, namely the A materials, were added through a special tool for later-added materials, arranged at a top end, and after the A materials were added, smelting was performed for 3-5 minutes after the power was regulated down to 300 KW so that the nucleation assisted alloys, namely the A materials, in the molten steel were softened but not in a free atom state completely. The molten steel was poured out when the temperature was in the range of 1410-1420° C. During pouring, the rotating speed of the copper roller wheel of the smelting furnace was about 40-45 r/min, the linear speed of the corresponding molten steel swinging position was 1.28-1.44 m/s, and casting strips with thicknesses of 0.15-0.35 mm were obtained.

(20) It can be seen from FIGS. 2A and 2B that after the nucleation assisted technique was adopted, the metallographic phase quality of the casting strips was improved, the tetragonal-phase columnar crystals were more sufficient in growth and better in penetration, and an increase of coercivity of magnets was facilitated.

(21) The Nd—Fe—B casting strips were then subjected to conventional crushing and powdering, pressing and forming, and sintering, so that the Nd—Fe—B finished products were obtained. A comparison table of properties of Nd—Fe—B finished products obtained by different technologies with the same ingredients is shown in the following Table 2. 2-1 # to 2-3 # shows the properties of the Nd—Fe—B magnets obtained by adopting the technique disclosed by the present disclosure, and 2-4 # to 2-6 # shows the properties of the Nd—Fe—B magnets obtained by adopting the traditional technology.

(22) TABLE-US-00002 TABLE 2 Comparison table of properties of Nd—Fe—B finished products obtained by different technologies with the same ingredients. (BH)max SN Br(T) Hcj(kAm/s) Hcb(kAm/s) (KJ/m3) Hk/Hcj 2-1# 1.387 1675 1075 370.5 0.991 2-2# 1.389 1669 1079 370.1 0.989 2-3# 1.391 1673 1080 372.6 0.990 2-4# 1.397 1548 1091 376.1 0.965 2-5# 1.396 1562 1089 375.6 0.962 2-6# 1.398 1563 1098 376.7 0.963

(23) It can be seen from FIGS. 2A and 2B and Table 2, after the technology and the technique were adopted, the metallographic phase quality of the casting strips was improved, the intrinsic coercivity Hcj of Nd—Fe—B finished products was improved, and residual magnetism was slightly reduced.