TW201624508A - NdFeB magnet and method for producing the same - Google Patents
NdFeB magnet and method for producing the same Download PDFInfo
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本發明係關於一種釹鐵硼磁體及其製造方法，特別是關於一種具有細小晶粒尺寸的釹鐵硼磁體及其製造方法。 The present invention relates to a neodymium iron boron magnet and a method of manufacturing the same, and more particularly to a neodymium iron boron magnet having a fine grain size and a method of manufacturing the same.
早期合金原料是採用冷卻速率較低的鑄錠塊材(Ingot)，合金中含有大量的α-Fe相，致使磁石產品特性不佳。雖然目前商用製程已改用冷卻速率稍快之甩片合金(Strip casting)以降低α-Fe相含量，但甩片合金之釹鐵硼主相或富稀土相之晶粒形狀為長條晶，晶粒尺寸之短軸約為0.1~50微米(μm)、長軸約0.1~100微米，侷限了甩片合金於後續氫破碎及氣流粉碎(Jet Mill)製程中的粉碎效果，其粉碎後粉體平均粒徑約1.5~5微米，致使燒結磁體之平均晶粒尺寸仍有5~15微米，晶粒略顯粗大導致磁石之本質矯頑磁力(iHc)、磁性值和耐溫性均不佳。 Early alloy materials used ingots with lower cooling rates (Ingot), which contained a large amount of α- Fe phase, resulting in poor magnetite properties. Although the commercial process has been changed to a slightly faster cooling strip alloy to reduce the α-Fe phase content, the grain shape of the NdFeB main phase or the rare earth-rich phase of the bismuth alloy is long-stranded. The short axis of the grain size is about 0.1 to 50 micrometers (μm) and the long axis is about 0.1 to 100 micrometers, which limits the pulverization effect of the bismuth alloy in the subsequent hydrogen crushing and Jet Mill process. The average particle size of the body is about 1.5~5 microns, so that the average grain size of the sintered magnet is still 5~15 microns. The grain size is slightly coarse, resulting in the intrinsic coercive force ( i H c ), magnetic value and temperature resistance of the magnet. .
例如，在美國專利公告第5,383,978號和中國專利公開第102031445A號中，均公開了針對燒結釹鐵硼磁石的製程，其係將熔融之釹鐵硼合金湯液澆鑄在高速旋轉的銅輪上，銅輪轉速約為2~4公尺/秒(m/s)，可製備出甩片合金。該甩片合金的冷卻速度約為103℃/秒，厚度約0.1~0.4毫米，合金中釹鐵硼主相或富稀土相之晶粒形狀為長條晶，晶粒尺 寸之短軸約0.1~50微米、長軸約0.1~300微米。該甩片合金經過氫粉碎和氣流粉碎之後，粉體的平均粒徑約為1.5~5微米，燒結後製得的燒結磁體之平均晶粒尺寸可控制在5~10微米左右。如上所述，在此晶粒範圍的燒結磁體，晶粒略顯粗大導致磁石磁性值有待改進。 For example, in the U.S. Patent No. 5,383,978 and the Chinese Patent Publication No. 102031445A, the process for sintering a neodymium-iron-boron magnet is disclosed in which a molten NdFeB alloy solution is cast on a high-speed rotating copper wheel. The copper wheel rotates at a speed of about 2 to 4 meters per second (m/s) to produce a bismuth alloy. The bismuth alloy has a cooling rate of about 10 3 ° C / sec and a thickness of about 0.1 to 0.4 mm. The grain shape of the NdFeB main phase or the rare earth-rich phase in the alloy is long-chain crystal, and the short axis of the grain size is about 0.1. ~50 microns, long axis about 0.1~300 microns. After the hydrogen pulverization and airflow pulverization of the bismuth alloy, the average particle diameter of the powder is about 1.5 to 5 μm, and the average grain size of the sintered magnet obtained after sintering can be controlled to about 5 to 10 μm. As described above, in the sintered magnet of this grain range, the crystal grains are slightly coarse, resulting in a magnetic value of the magnet to be improved.
故，有必要提供一種釹鐵硼磁體及其製造方法，可製得較小晶粒尺寸的釹鐵硼磁體，具有優良的磁性值，以解決習用技術所存在的問題。 Therefore, it is necessary to provide a neodymium iron boron magnet and a manufacturing method thereof, and a NdFeB magnet having a small grain size can be obtained, which has an excellent magnetic value to solve the problems of the conventional technology.
本發明之主要目的在於提供一種釹鐵硼磁體及其製造方法，可製得具有快速冷卻速率的釹鐵硼合金薄帶。該釹鐵硼合金薄帶在熱處理後，可獲得晶粒尺寸較小的釹鐵硼合金粉體，且其釹鐵硼主相或富稀土相為等軸晶粒(並非長短軸)。由於晶粒尺寸較小，在後續製程進行燒結或熱處理時所需溫度可降低，且燒結後所形成的磁體的磁性值相當優良。相較於傳統製程所製造的磁體，可提高約3~5千奧司特(kOe)的本質矯頑磁力。 SUMMARY OF THE INVENTION A primary object of the present invention is to provide a neodymium iron boron magnet and a method of manufacturing the same, which can produce a neodymium iron boron alloy ribbon having a rapid cooling rate. After the heat treatment, the NdFeB alloy ribbon can obtain a NdFeB alloy powder having a small grain size, and the NdFeB main phase or the rare earth-rich phase is an equiaxed grain (not a long axis). Due to the small grain size, the temperature required for sintering or heat treatment in subsequent processes can be lowered, and the magnetic properties of the magnet formed after sintering are quite excellent. Compared with the magnets manufactured by the conventional process, the intrinsic coercive force of about 3 to 5 kOe can be increased.
為達上述之目的，本發明的一實施例提供一種釹鐵硼磁體的製造方法，其主要包含步驟：將一釹鐵硼合金鑄塊粉碎後置於一石英管內，該石英管具有一噴嘴；加熱使該釹鐵硼合金鑄塊成為一熔融合金湯液；加壓使該熔融合金湯液從該噴嘴噴出並附著於一銅輪上，該銅輪的旋轉速率為30~45公尺/秒，冷卻後獲得一釹鐵硼合金薄帶；對該釹鐵硼合金薄帶進行熱處理；對該釹鐵硼合金薄帶進行氫破碎製程；對該釹鐵硼合金薄帶進行氣流粉碎製程，以形成一釹鐵硼合金粉體；對該釹鐵硼合金粉體進行 磁場成形配向處理；以及對該釹鐵硼合金粉體進行燒結和熱處理，以形成一釹鐵硼磁體。 In order to achieve the above object, an embodiment of the present invention provides a method for manufacturing a neodymium iron boron magnet, which mainly comprises the steps of: pulverizing a neodymium iron boron alloy ingot into a quartz tube having a nozzle; Heating to make the neodymium iron boron alloy ingot into a molten alloy soup; pressurizing the molten alloy soup solution from the nozzle and attaching to a copper wheel, the rotation speed of the copper wheel is 30 to 45 meters / After cooling, a thin band of NdFeB alloy is obtained after cooling; the NdFeB alloy strip is heat-treated; the NdFeB alloy strip is subjected to a hydrogen crushing process; and the NdFeB alloy strip is subjected to a jet milling process, Forming a niobium-iron-boron alloy powder; performing the niobium-iron-boron alloy powder Magnetic field forming alignment treatment; and sintering and heat treatment of the neodymium iron boron alloy powder to form a neodymium iron boron magnet.
在本發明之一實施例中，該釹鐵硼合金鑄塊之成份的化學式以重量百分比表示為：(Nd,Dy,Tb)xFeyCo2Cu0.2Nb0.2B1，其中27x30，x+y=96.6。 In one embodiment of the present invention, the chemical formula of the composition of the NdFeB alloy ingot is expressed by weight percentage: (Nd, Dy, Tb) x Fe y Co 2 Cu 0.2 Nb 0.2 B 1 , of which 27 x 30, x + y = 96.6.
在本發明之一實施例中，該熔融合金湯液係以高週波熔煉製得，其條件為：真空度5×10-5托(torr)，再通入氬氣至壓力560托。 In one embodiment of the present invention, the molten alloy soup solution is obtained by high-frequency melting, under the conditions of a vacuum of 5 × 10 -5 torr and then argon to a pressure of 560 torr.
在本發明之一實施例中，該熔融合金湯液係藉由通入氬氣至壓力760托，使該熔融合金湯液從該噴嘴噴出，噴嘴口徑0.6~0.9毫米(mm)。 In one embodiment of the present invention, the molten alloy soup solution is sprayed from the nozzle by passing argon gas to a pressure of 760 Torr, and the nozzle has a diameter of 0.6 to 0.9 mm.
在本發明之一實施例中，該釹鐵硼合金薄帶的冷卻速率為105~106℃/秒。 In an embodiment of the invention, the NdFeB alloy ribbon has a cooling rate of 10 5 to 10 6 ° C/sec.
在本發明之一實施例中，該釹鐵硼合金薄帶的熱處理條件為：溫度500~700℃，持續10~60分鐘。 In an embodiment of the present invention, the heat treatment condition of the NdFeB alloy ribbon is: a temperature of 500 to 700 ° C for 10 to 60 minutes.
在本發明之一實施例中，該釹鐵硼合金薄帶的氫破碎製程條件為：吸氫壓力1.8~2.5千克力/平方公分(kgf/cm2)，維持1~3小時。 In one embodiment of the present invention, the hydrogen crushing process condition of the NdFeB alloy ribbon is: hydrogen absorption pressure of 1.8 to 2.5 kgf/cm 2 (kgf/cm 2 ) for 1 to 3 hours.
在本發明之一實施例中，在該釹鐵硼合金薄帶的氫破碎製程中，脫氫溫度為450~650℃，維持1~3小時。 In one embodiment of the present invention, in the hydrogen crushing process of the NdFeB alloy ribbon, the dehydrogenation temperature is 450 to 650 ° C for 1 to 3 hours.
在本發明之一實施例中，在該釹鐵硼合金薄帶的氣流粉碎製程中，壓力為0.3~0.5兆帕，分級輪轉速為4800~5000轉/分鐘(rpm)。 In an embodiment of the present invention, in the airflow pulverization process of the NdFeB alloy ribbon, the pressure is 0.3-0.5 MPa, and the grading wheel rotation speed is 4800-5000 rpm.
在本發明之一實施例中，該釹鐵硼合金粉體的粒徑為1~2微米(μm)。 In an embodiment of the invention, the NdFeB alloy powder has a particle size of 1 to 2 micrometers (μm).
在本發明之一實施例中，該燒結條件為：真空度5×10-5托，溫度900~1000℃，持續3小時。 In one embodiment of the invention, the sintering conditions are: a vacuum of 5 x 10 -5 Torr and a temperature of 900 to 1000 ° C for 3 hours.
在本發明之一實施例中，對該釹鐵硼合金粉體進行該熱處理的條件為：真空度5×10-5托，溫度700~800℃，持續2小時。 In an embodiment of the present invention, the heat treatment is performed on the neodymium iron boron alloy powder under the conditions of a vacuum of 5 × 10 -5 Torr and a temperature of 700 to 800 ° C for 2 hours.
本發明的再一實施例提供一種釹鐵硼磁體，其係以上述製造方法所製得，其具有晶粒平均尺寸為2~4微米。 Still another embodiment of the present invention provides a neodymium iron boron magnet obtained by the above-described manufacturing method, which has an average crystal grain size of 2 to 4 μm.
S1、S2、S3、S4、S5、S6、S7、S8‧‧‧步驟 S1, S2, S3, S4, S5, S6, S7, S8‧‧
11‧‧‧石英管 11‧‧‧Quartz tube
12‧‧‧氣體通道 12‧‧‧ gas passage
13‧‧‧加熱線圈 13‧‧‧heating coil
14‧‧‧銅輪 14‧‧‧Bronze wheel
21‧‧‧熔融合金湯液 21‧‧‧ molten alloy soup
22‧‧‧釹鐵硼合金薄帶 22‧‧‧NdFeB alloy strip
111‧‧‧噴嘴 111‧‧‧Nozzles
第1圖：本發明一實施例之釹鐵硼磁體的製造方法的流程示意圖。 Fig. 1 is a flow chart showing a method of producing a neodymium iron boron magnet according to an embodiment of the present invention.
第2圖：本發明一實施例之釹鐵硼磁體的製造方法所使用之裝置示意圖。 Fig. 2 is a view showing the apparatus used in the method for producing a neodymium iron boron magnet according to an embodiment of the present invention.
為了讓本發明之上述及其他目的、特徵、優點能更明顯易懂，下文將特舉本發明較佳實施例，並配合所附圖式，作詳細說明如下。再者，本發明所提到的單數形式“一”、“一個”和“所述”包括複數引用，除非上下文另有明確規定。例如，術語“一化合物”或“至少一種化合物”可以包括多個化合物，包括其混合物；本發明文中提及的「%」若無特定說明皆指「重量百分比(wt%)」；數值範圍(如10%~11%的A)若無特定說明皆包含上、下限值(即10%≦A≦11%)；數值範圍若未界定下限值(如低於0.2%的B，或0.2%以下的B)，則皆指其下限值可能為0(即0%≦B≦0.2%)；各成份的「重量百分比」之比例關係亦可置換為「重量份」的比例關係。上述用語是用以說明及理解本發明，而非用以限制本發明。 The above and other objects, features and advantages of the present invention will become more <RTIgt; In addition, the singular forms "a," "," For example, the term "a compound" or "at least one compound" may include a plurality of compounds, including mixtures thereof; "%" as referred to in the present specification means "percent by weight (wt%)" unless otherwise specified; For example, 10%~11% of A) include upper and lower limits (ie 10% ≦A≦11%) unless otherwise specified; if the value range does not define a lower limit (such as B below 0.2%, or 0.2) B) below B) means that the lower limit may be 0 (ie 0% ≦ B ≦ 0.2%); the proportional relationship of the "weight percentage" of each component may also be replaced by the proportional relationship of "parts by weight". The above terms are used to illustrate and understand the present invention and are not intended to limit the invention.
請參考第1圖，本發明一實施例提供一種釹鐵硼磁體的製造方法，其主要包括步驟：(S1)將一釹鐵硼合金鑄塊粉碎後，置於一石英管內；(S2)加熱成為一熔融合金湯液；(S3)噴出該熔融合金湯液於一銅輪上，冷卻後獲得一釹鐵硼合金薄帶；(S4)對該釹鐵硼合金薄帶進行熱處理；(S5)對該釹鐵硼合金薄帶進行氫破碎製程；(S6)對該釹鐵硼合金薄帶進行氣流粉碎製程，以形成一釹鐵硼合金粉體；(S7)對該釹鐵硼合金粉體進行磁場成形配向處理；以及(S8)對該釹鐵硼合金粉體進行燒結和熱處理，以形成一釹鐵硼磁體。本發明將於下文逐一詳細說明該實施例之上述各步驟的實施細節及其原理。 Referring to FIG. 1 , an embodiment of the present invention provides a method for manufacturing a neodymium iron boron magnet, which mainly includes the steps of: (S1) pulverizing a neodymium iron boron alloy ingot and placing it in a quartz tube; (S2) Heating into a molten alloy soup solution; (S3) spraying the molten alloy soup liquid on a copper wheel, cooling to obtain a tantalum-iron-boron alloy ribbon; (S4) heat-treating the NdFeB alloy ribbon; (S5) (S6) performing a hydrogenation process on the NdFeB alloy ribbon; (S6) performing a jet milling process on the NdFeB alloy ribbon to form a NdFeB alloy powder; (S7) the NdFeB alloy powder The body is subjected to a magnetic field forming alignment treatment; and (S8) the neodymium iron boron alloy powder is sintered and heat treated to form a neodymium iron boron magnet. The details of the implementation of the above-described steps of the embodiment and the principles thereof will be described in detail below.
請參考第1至2圖，本發明一實施例之釹鐵硼磁體的製造方法首先係：(S1)將一釹鐵硼合金鑄塊粉碎後，置於一石英管11內。在本步驟中，該石英管11具有一噴嘴111。該釹鐵硼合金鑄塊之成份之化學式若以重量百分比表示可例如是：(Nd,Dy,Tb)xFeyCo2Cu0.2Nb0.2B1，其中27x30，x+y=96.6，也就是總稀土重量(Nd,Dy,Tb)佔該釹鐵硼合金鑄塊27~30wt%之間。例如當總稀土重量為28wt%時，鐵則佔約68.6wt%，然不限於此。該釹鐵硼合金鑄塊粉碎後的尺寸大小並不限制，可視實際操作時該石英管11的尺寸調整，只要可以順利置入即可。 Referring to FIGS. 1 to 2, a method for manufacturing a neodymium iron boron magnet according to an embodiment of the present invention is first: (S1) pulverizing a neodymium iron boron alloy ingot and placing it in a quartz tube 11. In this step, the quartz tube 11 has a nozzle 111. The chemical formula of the composition of the NdFeB alloy ingot may be, for example, by weight percentage: (Nd, Dy, Tb) x Fe y Co 2 Cu 0.2 Nb 0.2 B 1 , of which 27 x 30, x + y = 96.6, that is, the total rare earth weight (Nd, Dy, Tb) accounts for 27 to 30% by weight of the NdFeB alloy ingot. For example, when the total rare earth weight is 28% by weight, iron accounts for about 68.6 wt%, but is not limited thereto. The size of the NdFeB alloy ingot after pulverization is not limited, and the size of the quartz tube 11 can be adjusted as long as it can be smoothly placed.
本發明一實施例之釹鐵硼磁體的製造方法接著係：(S2)加熱成為一熔融合金湯液21。在此步驟中，該熔融合金湯液21可例如是以高週波熔煉製得，其條件為：真空度5×10-5托(torr)，再通入氬氣至壓力560托。此外，在一加熱線圈13作用之下，加熱至該釹鐵硼合金鑄塊到達熔點(該壓力下)，可例如是1350℃，形成該熔融合金湯液21。 A method for producing a neodymium iron boron magnet according to an embodiment of the present invention is followed by heating (S2) to form a molten alloy soup solution 21. In this step, the molten alloy soup solution 21 can be obtained, for example, by high-frequency melting, under the conditions of a vacuum of 5 × 10 -5 torr, and then argon gas to a pressure of 560 Torr. Further, under the action of the heating coil 13, heating to the NdFeB alloy ingot to reach the melting point (at this pressure) may be, for example, 1350 ° C to form the molten alloy soup solution 21.
本發明一實施例之釹鐵硼磁體的製造方法接著係：(S3)噴出該熔融合金湯液21於一銅輪14上，冷卻後獲得一釹鐵硼合金薄帶。在本步驟中，該熔融合金湯液係藉由從一氣體通道12通入氬氣至壓力760托，由於該石英管內外壓力差，使得該熔融合金湯液21從該噴嘴111噴出，該噴嘴111之口徑為0.6~0.9毫米。該銅輪14由於該銅輪14的旋轉速率為30~45公尺/秒，可例如是35、40或45公尺/秒，然不限於此。藉由該銅輪14旋轉時可提供被噴出的該熔融合金湯液21初步的冷卻效果，被冷卻的該熔融合金湯液21可形成一釹鐵硼合金薄帶22，具有冷卻速率約為105~106℃/秒。 A method for producing a neodymium iron boron magnet according to an embodiment of the present invention is followed by: (S3) spraying the molten alloy soup solution 21 onto a copper wheel 14, and cooling to obtain a NdFeB alloy ribbon. In this step, the molten alloy soup liquid is ejected from the gas passage 12 to the pressure of 760 Torr, and the molten alloy soup solution 21 is ejected from the nozzle 111 due to the pressure difference between the inside and outside of the quartz tube. The diameter of 111 is 0.6~0.9 mm. The copper wheel 14 can be, for example, 35, 40 or 45 meters/second because the rotation speed of the copper wheel 14 is 30 to 45 meters/second, but is not limited thereto. The initial cooling effect of the molten alloy soup solution 21 can be provided by the rotation of the copper wheel 14, and the cooled molten alloy soup solution 21 can form a neodymium iron boron alloy ribbon 22 having a cooling rate of about 10 5 ~ 10 6 °C / sec.
本發明一實施例之釹鐵硼磁體的製造方法接著係：(S4)對該釹鐵硼合金薄帶22進行熱處理。該釹鐵硼合金薄帶22的熱處理條件可為：溫度500~700℃，持續10~60分鐘，可例如是在溫度700℃進行30分鐘，或是在溫度600℃進行60分鐘，然不限於此。 A method for producing a neodymium iron boron magnet according to an embodiment of the present invention is followed by: (S4) heat treatment of the neodymium iron boron alloy ribbon 22. The heat treatment condition of the NdFeB strip 22 may be: a temperature of 500 to 700 ° C for 10 to 60 minutes, and may be, for example, 30 minutes at a temperature of 700 ° C or 60 minutes at a temperature of 600 ° C, but is not limited thereto. this.
本發明一實施例之釹鐵硼磁體的製造方法接著係：(S5)對該釹鐵硼合金薄帶22進行氫破碎製程。在本步驟中，可在一惰性氣體環境下進行，例如通入氬氣。該釹鐵硼合金薄帶22的氫破碎製程條件可為：吸氫壓力1.8~2.5千克力/平方公分(kgf/cm2)，維持1~3小時，可例如是在吸氫壓力1.9千克力/平方公分進行2小時，然不限於此。此外，在該釹鐵硼合金薄帶22的氫破碎製程中，其脫氫溫度可為450~650℃，維持1~3小時，可例如是在脫氫溫度550℃中持續1小時。 A method for producing a neodymium iron boron magnet according to an embodiment of the present invention is followed by: (S5) performing a hydrogen crushing process on the neodymium iron boron alloy ribbon 22. In this step, it can be carried out under an inert gas atmosphere, for example, by introducing argon gas. The hydrogen crushing process condition of the NdFeB strip 22 can be: hydrogen absorption pressure of 1.8 to 2.5 kgf/cm 2 (kgf/cm 2 ), maintained for 1 to 3 hours, for example, at a hydrogen absorption pressure of 1.9 kg. / square centimeter for 2 hours, but not limited to this. In addition, in the hydrogen crushing process of the NdFeB strip 22, the dehydrogenation temperature may be 450 to 650 ° C for 1 to 3 hours, for example, at a dehydrogenation temperature of 550 ° C for 1 hour.
本發明一實施例之釹鐵硼磁體的製造方法接著係：(S6)對該釹鐵硼合金薄帶22進行氣流粉碎製程，以形成一釹鐵硼合金粉體。在本 步驟中，該釹鐵硼合金薄帶22的氣流粉碎製程條件為：壓力0.3~0.5兆帕(MPa)，分級輪轉速為4800~5000轉/分鐘(rpm)，可例如壓力0.5兆帕，分級輪轉速為5000轉/分鐘，然不限於此。進行粉碎後，該釹鐵硼合金粉體的粒徑可被細化至約為1~2微米(μm)。 A method for producing a neodymium iron boron magnet according to an embodiment of the present invention is followed by: (S6) performing a jet milling process on the neodymium iron boron alloy ribbon 22 to form a neodymium iron boron alloy powder. In this In the step, the air flow pulverization process condition of the NdFeB strip 22 is: a pressure of 0.3 to 0.5 MPa, and a grading wheel rotation speed of 4800 to 5000 rpm, which can be, for example, a pressure of 0.5 MPa. The wheel speed is 5000 rpm, but it is not limited to this. After the pulverization, the particle size of the NdFeB alloy powder can be refined to about 1 to 2 μm.
接著，依照本發明一實施例之釹鐵硼磁體的製造方法中，在形成該釹鐵硼合金粉體之後，接著係(S7)：對該釹鐵硼合金粉體進行磁場成形配向處理，以使該釹鐵硼合金粉體具備一磁性方向；以及於磁場成形配向後(S8)：對該釹鐵硼合金粉體進行燒結和熱處理，以形成一釹鐵硼磁體。在一實施例中，該燒結條件可為：真空度5×10-5托，溫度900~1000℃，持續3小時，例如是真空狀態中，溫度為950℃，燒結3小時，然不限於此。此外，對該該釹鐵硼合金粉體進行熱處理的條件可為：真空度5×10-5托，溫度700~800℃，持續2小時，可例如是真空狀態中，溫度為750℃，燒結2小時，然不限於此。所製得的該釹鐵硼磁體經測定後，本質矯頑磁力可較傳統製程提升3~5千奧司特。該釹鐵硼磁體的晶粒平均尺寸為2~4微米，可例如是2.3、3.2或3.8微米，然不限於此。 Next, in the method for producing a neodymium iron boron magnet according to an embodiment of the present invention, after the formation of the neodymium iron boron alloy powder, followed by a system (S7): performing magnetic field forming alignment treatment on the neodymium iron boron alloy powder to The neodymium iron boron alloy powder is provided with a magnetic direction; and after the magnetic field forming alignment (S8): the neodymium iron boron alloy powder is sintered and heat treated to form a neodymium iron boron magnet. In one embodiment, the sintering condition may be: a degree of vacuum of 5×10 −5 Torr, a temperature of 900 to 1000° C. for 3 hours, for example, a vacuum state, a temperature of 950° C., and sintering for 3 hours, but is not limited thereto. . In addition, the heat treatment condition of the NdFeB alloy powder may be: a vacuum degree of 5×10 −5 Torr, a temperature of 700 to 800° C. for 2 hours, for example, a vacuum state, a temperature of 750° C., sintering 2 hours, it is not limited to this. After the prepared NdFeB magnet is measured, the intrinsic coercive force can be increased by 3~5 kAs in comparison with the conventional process. The NdFeB magnet has an average grain size of 2 to 4 μm and may be, for example, 2.3, 3.2 or 3.8 μm, but is not limited thereto.
為使本發明之釹鐵硼磁體的製造方法更明確，請參考下文所述之實際製造流程。然所述製造方式僅為範例，並非用於限制該釹鐵硼磁體的結構及其製造步驟。 In order to clarify the manufacturing method of the NdFeB magnet of the present invention, please refer to the actual manufacturing process described below. However, the manufacturing method is merely an example, and is not intended to limit the structure of the neodymium iron boron magnet and the manufacturing steps thereof.
首先，將重量約為2公斤之Nd26.5Dy4.5Fe65.6Co2Cu0.2Nb0.2B1合金鑄錠塊敲碎成適當體積後，置入石英管11中(請參考第1圖)，並將石英管11置入一真空腔體(未繪示)內。石英管11之噴嘴111口徑為0.8毫米，噴嘴111至銅輪14表面之距離為6毫米。在真空腔體內之真空度達 到5×10-5托之後，通入氬氣使腔體壓力升高至560托。接著開啟高週波熔煉，使鑄錠塊成為熔融湯液後，從氣體通道12通入760托氬氣於石英管111中，使熔融湯液自石英管下方之噴嘴111迅速噴出於高速旋轉的銅輪面上。銅輪轉速設定為40公尺/秒，合金薄帶所具備之冷卻速度約105~106℃/秒，製得合金薄帶厚度約為0.01~0.03毫米。 First, a Nd 26.5 Dy 4.5 Fe 65.6 Co 2 Cu 0.2 Nb 0.2 B 1 alloy ingot having a weight of about 2 kg is broken into an appropriate volume and placed in a quartz tube 11 (please refer to FIG. 1), and The quartz tube 11 is placed in a vacuum chamber (not shown). The nozzle 111 of the quartz tube 11 has a diameter of 0.8 mm, and the distance from the nozzle 111 to the surface of the copper wheel 14 is 6 mm. After the vacuum in the vacuum chamber reached 5 × 10 -5 Torr, argon gas was introduced to raise the chamber pressure to 560 Torr. Then, the high-frequency smelting is started, and after the ingot is melted, the argon gas is introduced into the quartz tube 111 from the gas passage 12, and the molten soup is quickly sprayed from the nozzle 111 below the quartz tube to the high-speed rotating copper. On the wheel. The copper wheel speed is set to 40 meters / sec, the alloy ribbon has a cooling rate of about 105 ~ 106 ° C / sec, and the thickness of the alloy strip is about 0.01 ~ 0.03 mm.
接著，將製得的合金薄帶至於真空腔體內(真空度5×10-5托)進行熱處理，熱處理條件為700℃×30分鐘。合金薄帶熱處理後晶粒尺寸約0.1~3微米，呈現主要為釹鐵硼主相與富稀土相。將熱處理後之合金薄帶在氬氣保護下進行氫破碎製程。氫破碎之吸氫壓力為1.95公斤力/平方公分，維持2小時；脫氫溫度為550℃，持續1小時。接著再將氫破碎後的釹鐵硼合金粉體，在氮氣保護下進行氣流粉碎，氣流粉碎的壓力為0.5兆帕，分級輪轉速為5000轉/分鐘。經過氣流粉碎後之釹鐵硼合金粉體的平均粒徑尺寸可細化至1~2微米。 Next, the obtained alloy ribbon was subjected to heat treatment in a vacuum chamber (vacuum degree: 5 × 10 -5 Torr) under heat treatment conditions of 700 ° C × 30 minutes. After heat treatment, the alloy ribbon has a grain size of about 0.1~3 microns, which is mainly composed of NdFeB main phase and rare earth-rich phase. The heat-treated alloy ribbon is subjected to a hydrogen fragmentation process under argon gas protection. The hydrogen absorption pressure of hydrogen fragmentation was 1.95 kgf/cm 2 for 2 hours; the dehydrogenation temperature was 550 ° C for 1 hour. Then, the NdFeB alloy powder after the hydrogen was crushed was subjected to jet pulverization under a nitrogen atmosphere, and the pressure of the jet pulverization was 0.5 MPa, and the grading wheel rotation speed was 5000 rpm. The average particle size of the NdFeB alloy powder after jet milling can be refined to 1 to 2 microns.
接著，該釹鐵硼合金粉體經過磁場成形配向後，置入真空燒結爐中進行燒結及熱處理。所使用的燒結條件為950℃×3小時，真空度5×10-5托；熱處理條件為750℃×2小時，真空度5×10-5托。燒結後，獲得一釹鐵硼磁體，其具有平均晶粒尺寸約2.4微米，磁石之本質矯頑磁力相較於傳統製程提昇了3.6千奧司特，。本實施例中，該釹鐵硼磁體的磁性值請參考下表1。 Next, the NdFeB alloy powder is subjected to magnetic field forming and then placed in a vacuum sintering furnace for sintering and heat treatment. The sintering conditions used were 950 ° C × 3 hours, the degree of vacuum was 5 × 10 -5 Torr, the heat treatment conditions were 750 ° C × 2 hours, and the degree of vacuum was 5 × 10 -5 Torr. After sintering, a neodymium iron boron magnet having an average grain size of about 2.4 μm was obtained, and the intrinsic coercive force of the magnet was increased by 3.6 kOs compared to the conventional process. In this embodiment, the magnetic properties of the neodymium iron boron magnet are as shown in Table 1 below.
Br：殘留磁化量、iHc：本質矯頑磁力、(BH)max：磁能積 Br: residual magnetization, iHc: intrinsic coercive force, (BH) max : magnetic energy product
如表1所示，燒結前的粉體粒徑約為1.8微米，相較於傳統製程(比較例)中的粉體粒徑2.8微米已有明顯的細緻化。而燒結後所形成的該釹鐵硼磁體之晶粒尺寸約為2.9微米，遠小於比較例中的晶粒尺寸。此外，實施例中該釹鐵硼磁體所具有的磁石之本質矯頑磁力為27.1千奧司特，相較於比較例的23.5千奧司特，確實有大幅度的提昇。 As shown in Table 1, the powder particle size before sintering was about 1.8 μm, which was significantly finer than the powder particle size of 2.8 μm in the conventional process (Comparative Example). The grain size of the NdFeB magnet formed after sintering is about 2.9 μm, which is much smaller than the grain size in the comparative example. Further, in the embodiment, the magnetron of the neodymium iron boron magnet has an intrinsic coercive force of 27.1 kA, which is a substantial improvement compared to the 23.5 kOs of the comparative example.
相較於習知技術，依照本發明所提供之釹鐵硼磁體的製造方法中，利用具有快速冷卻速率的釹鐵硼合金薄帶，使該釹鐵硼合金薄帶在熱處理後，獲得粒徑較小的釹鐵硼合金粉體，且其釹鐵硼主相或富稀土相為等軸晶粒。由於粒徑較小，在後續製程進行燒結或熱處理時形成燒結磁體時，所需溫度可降低，且所形成的釹鐵硼磁體的晶粒尺寸遠小於傳統製程，且磁性值相當優良，本質矯頑磁力可以提昇3~5千奧司特。 Compared with the prior art, in the method for manufacturing a neodymium iron boron magnet according to the present invention, the NdFeB alloy ribbon having a rapid cooling rate is used to obtain the particle size of the NdFeB alloy ribbon after heat treatment. A smaller NdFeB alloy powder, and its NdFeB main phase or rare earth-rich phase is an equiaxed grain. Due to the small particle size, when a sintered magnet is formed during sintering or heat treatment in a subsequent process, the required temperature can be lowered, and the grain size of the formed NdFeB magnet is much smaller than that of the conventional process, and the magnetic value is quite excellent. The coercive force can be increased by 3~5 thousand Åtes.
雖然本發明已以較佳實施例揭露，然其並非用以限制本發明，任何熟習此項技藝之人士，在不脫離本發明之精神和範圍內，當可作各種更動與修飾，因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。 The present invention has been disclosed in its preferred embodiments, and is not intended to limit the invention, and the present invention may be modified and modified without departing from the spirit and scope of the invention. The scope of protection is subject to the definition of the scope of the patent application.
S1、S2、S3、S4、S5、S6、S7、S8‧‧‧步驟 S1, S2, S3, S4, S5, S6, S7, S8‧‧
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