TW202108782A - Ndfeb permanent magnet material and raw material composition, preparation method and application thereof - Google Patents
Ndfeb permanent magnet material and raw material composition, preparation method and application thereof Download PDFInfo
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- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
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- H01F41/02—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
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- H01F41/00—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
- H01F41/02—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
- 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
- H01F41/0266—Moulding; Pressing
Abstract
Description
本發明係有關一種釹鐵硼永磁材料及其原料組合物、製備方法和應用。The invention relates to a neodymium iron boron permanent magnet material and its raw material composition, preparation method and application.
燒結釹鐵硼以其優異的磁性能,廣泛用於動力電機、計算機及電子產品等領域,隨著產品的迭代,這些領域對磁體的溫度係數提出更高的要求。Sintered NdFeB is widely used in the fields of power motors, computers and electronic products due to its excellent magnetic properties. With the iteration of products, these fields put forward higher requirements on the temperature coefficient of magnets.
目前燒結釹鐵硼的磁通溫度係數α約為-0.11%/°C至-0.14%/°C,而燒結釤鈷產品的磁通溫度係數α可達-0.04%/°C。可見,燒結釹鐵硼的磁通溫度係數的絕對值遠高於燒結釤鈷的磁通溫度係數的絕對值,這一性能上的缺陷限制了燒結釹鐵硼產品的應用範圍。At present, the magnetic flux temperature coefficient α of sintered NdFeB is about -0.11%/°C to -0.14%/°C, while the magnetic flux temperature coefficient α of sintered samarium cobalt products can reach -0.04%/°C. It can be seen that the absolute value of the magnetic flux temperature coefficient of sintered NdFeB is much higher than that of sintered samarium cobalt. This performance defect limits the application range of sintered NdFeB products.
為了降低燒結釹鐵硼磁體的磁通溫度係數的絕對值,大部分釹鐵硼生產廠家一般採用以下兩種方式:In order to reduce the absolute value of the magnetic flux temperature coefficient of sintered NdFeB magnets, most NdFeB manufacturers generally adopt the following two methods:
A. 通過添加大量的Co來提高磁體的居禮溫度。但是Co在釹鐵硼中的新增量>8%時,才能獲得釹鐵硼的磁通溫度係數α為-0.06%/°C的效果。該方式成本較高,且Co在該添加量下會導致釹鐵硼的內稟矯頑力(intrinsic coercivity,簡稱Hcj)的下降。A. Increase the Curie temperature of the magnet by adding a large amount of Co. However, when the newly added amount of Co in NdFeB is more than 8%, the effect that the temperature coefficient of magnetic flux α of NdFeB is -0.06%/°C can be obtained. The cost of this method is relatively high, and the addition of Co will cause a decrease in the intrinsic coercivity (Hcj) of the neodymium iron boron.
B. 通過添加大量Pr、Nd、Dy、Tb等稀土元素來提高磁體的內稟矯頑力。在Dy、Tb的新增量大於5 wt.%時,能夠獲得釹鐵硼的磁通溫度係數α為-0.09%/°C的效果。但是,該方式顯著增加了生產成本,且會導致釹鐵硼的剩磁的下降。B. Increase the intrinsic coercivity of the magnet by adding a large amount of rare earth elements such as Pr, Nd, Dy, and Tb. When the newly added amount of Dy and Tb is greater than 5 wt.%, the effect that the temperature coefficient of magnetic flux α of NdFeB is -0.09%/°C can be obtained. However, this method significantly increases the production cost and causes the remanence of the neodymium iron boron to decrease.
因此,如何在保持釹鐵硼永磁材料的內稟矯頑力和剩磁的基礎上,提供一種低磁通溫度係數的釹鐵硼永磁材料,是本領域亟待解決的技術問題。Therefore, how to provide a neodymium iron boron permanent magnet material with a low magnetic flux temperature coefficient on the basis of maintaining the intrinsic coercivity and remanence of the neodymium iron boron permanent magnetic material is an urgent technical problem in this field.
本發明所要解決的技術問題在於,克服現有技術中由於釹鐵硼的磁通溫度係數的絕對值過高,難以滿足動力電機、計算機及電子產品等精密儀器的性能要求的缺陷,而提供了一種釹鐵硼永磁材料及其原料組合物、製備方法和應用。The technical problem to be solved by the present invention is to overcome the defect that the absolute value of the magnetic flux temperature coefficient of neodymium iron boron in the prior art is too high, and it is difficult to meet the performance requirements of precision instruments such as power motors, computers and electronic products, and to provide a Neodymium iron boron permanent magnet material and its raw material composition, preparation method and application.
本發明通過精確的配方設計,使得釹鐵硼永磁材料的原料中Nb含量≧0.3%wt以及Ga含量≧0.1%,從而製得了一種低溫度係數的釹鐵硼永磁材料,該釹鐵硼永磁材料在20°C~100°C溫度區間的磁通溫度係數α的絕對值≦0.085%/°C。The invention makes the Nb content ≧0.3%wt and the Ga content ≧0.1% in the raw materials of the neodymium iron boron permanent magnet material through precise formulation design, thereby preparing a neodymium iron boron permanent magnet material with a low temperature coefficient. The absolute value of the magnetic flux temperature coefficient α of the permanent magnet material in the temperature range of 20°C to 100°C is ≦0.085%/°C.
本發明提供了一種釹鐵硼永磁材料,其包含下述組分:Nd為24.0~29.0%、RH為3.0~6.0%、Cu為0.1~0.3%、Co為1.0~4.0%、Ga為0.1~0.6%、Nb為0.3~0.5%、Ti為0.0~0.3%和B為0.90~1.02%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比;所述RH為重稀土元素。The present invention provides a neodymium iron boron permanent magnet material, which contains the following components: Nd is 24.0-29.0%, RH is 3.0-6.0%, Cu is 0.1-0.3%, Co is 1.0-4.0%, and Ga is 0.1 ~0.6%, Nb is 0.3~0.5%, Ti is 0.0~0.3% and B is 0.90~1.02%, the balance is Fe and inevitable impurities, the percentage refers to the mass in the neodymium iron boron permanent magnet material Percentage; The RH is a heavy rare earth element.
本發明中,所述Nd的含量優選為25.5~28.5%或25.5~27.5%,例如25.5%、26.0%、27.5%或28.5%,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In the present invention, the Nd content is preferably 25.5-28.5% or 25.5-27.5%, such as 25.5%, 26.0%, 27.5% or 28.5%, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material .
本發明中,所述RH可為本領域常規的重稀土元素,例如Dy和/或Tb,優選為Dy。In the present invention, the RH may be a heavy rare earth element conventional in the art, such as Dy and/or Tb, preferably Dy.
本發明中,所述RH的含量優選為4.0~6.0%或4.0~5.5%,例如4.0%、5.5%或6.0%,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In the present invention, the RH content is preferably 4.0-6.0% or 4.0-5.5%, such as 4.0%, 5.5% or 6.0%, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
本發明中,所述Cu的含量優選為0.1~0.2%,例如0.1%、0.15%或0.2%,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In the present invention, the content of Cu is preferably 0.1% to 0.2%, such as 0.1%, 0.15% or 0.2%, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
本發明中,所述Co的含量優選為1.0~3.0%或1.0~2.0%,例如1.0%、2.0%或2.5%,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In the present invention, the content of Co is preferably 1.0-3.0% or 1.0-2.0%, such as 1.0%, 2.0% or 2.5%, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
本發明中,所述Ga的含量優選為0.15~0.6%或0.15~0.5%,例如0.15%、0.2%、0.3%、0.35%、0.45%、0.5%或0.6%,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In the present invention, the content of Ga is preferably 0.15~0.6% or 0.15~0.5%, such as 0.15%, 0.2%, 0.3%, 0.35%, 0.45%, 0.5% or 0.6%, and the percentage refers to the content of the neodymium The mass percentage of iron-boron permanent magnet materials.
本發明中,所述Nb的含量優選為0.3~0.4%或0.3~0.35%,例如0.3%、0.35%或0.4%,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In the present invention, the Nb content is preferably 0.3-0.4% or 0.3-0.35%, such as 0.3%, 0.35% or 0.4%, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
本發明中,所述Ti的含量優選為0.1~0.3%或0.1~0.2%,例如0.15%、0.2%或0.3%,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In the present invention, the content of Ti is preferably 0.1-0.3% or 0.1-0.2%, such as 0.15%, 0.2% or 0.3%, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
本發明中,所述B的含量優選為0.92~1.02%,例如0.95%,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In the present invention, the content of B is preferably 0.92 to 1.02%, such as 0.95%, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
本發明中,優選地,所述Ga的含量為0.15~0.6%,所述Nb的含量為0.3~0.4%;更優選地,所述Ga的含量為0.15~0.5%,所述Nb的含量為0.3~0.35%;例如,Ga為0.20%、Nb為0.3%,Ga為0.35%、Nb為0.4%,Ga為0.45%,Nb為0.5%,Ga為0.5%、Nb 為0.5%,Ga為0.6%、Nb為0.3%,Ga為0.5%、Nb為0.35%、Ga為0.3% 、Nb為0.4%,或者,Ga為0.15%、Nb為0.5%;百分比是指在所述釹鐵硼永磁材料中的質量百分比。In the present invention, preferably, the content of Ga is 0.15 to 0.6%, and the content of Nb is 0.3 to 0.4%; more preferably, the content of Ga is 0.15 to 0.5%, and the content of Nb is 0.3~0.35%; For example, Ga is 0.20%, Nb is 0.3%, Ga is 0.35%, Nb is 0.4%, Ga is 0.45%, Nb is 0.5%, Ga is 0.5%, Nb is 0.5%, Ga is 0.6 %, Nb is 0.3%, Ga is 0.5%, Nb is 0.35%, Ga is 0.3%, Nb is 0.4%, or Ga is 0.15%, Nb is 0.5%; the percentage refers to the neodymium iron boron permanent magnet The mass percentage in the material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為25.5~28.5%、Dy為4.0~6.0%、Cu為0.1~0.2%、Co為1.0~3.0%、Ga為0.15~0.6%、Nb為0.3~0.4%、Ti為0.1~0.3%和B為0.92~1.02%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material contains the following components: Nd is 25.5-28.5%, Dy is 4.0-6.0%, Cu is 0.1-0.2%, and Co is 1.0-3.0% , Ga is 0.15~0.6%, Nb is 0.3~0.4%, Ti is 0.1~0.3% and B is 0.92~1.02%, the balance is Fe and unavoidable impurities, the percentage refers to the said neodymium iron boron permanent magnet The mass percentage in the material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為25.5~27.5%、Dy為4.0~5.5%、Cu為0.1~0.2%、Co為1.0~2.0%、Ga為0.15~0.5%、Nb 為0.3~0.35%、Ti為0.1~0.2%和B為0.92~1.02%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material contains the following components: Nd is 25.5~27.5%, Dy is 4.0~5.5%, Cu is 0.1~0.2%, Co is 1.0~2.0% , Ga is 0.15~0.5%, Nb is 0.3~0.35%, Ti is 0.1~0.2% and B is 0.92~1.02%, the balance is Fe and inevitable impurities, the percentage refers to the said neodymium iron boron permanent magnet The mass percentage in the material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為27.5%、Dy為4.0%、Cu為0.2%、Co為2.5%、Ga為0.20%、Nb為0.3%、Ti為0.15%和B為0.95%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material comprises the following components: Nd is 27.5%, Dy is 4.0%, Cu is 0.2%, Co is 2.5%, Ga is 0.20%, and Nb is 0.3%, 0.15% for Ti and 0.95% for B, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為27.5%、Dy為4.0%、Cu為0.2%、Co為2.5%、Ga為0.35%、Nb為0.4%、Ti為0.15%和B為0.95%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material comprises the following components: Nd is 27.5%, Dy is 4.0%, Cu is 0.2%, Co is 2.5%, Ga is 0.35%, and Nb is 0.4%, Ti is 0.15%, and B is 0.95%, the balance is Fe and inevitable impurities, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為27.5%、Dy為4.0%、Cu為0.2%、Co為2.5%、Ga為0.45%、Nb為0.5%、Ti為0.15%和B為0.95%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material contains the following components: Nd is 27.5%, Dy is 4.0%, Cu is 0.2%, Co is 2.5%, Ga is 0.45%, and Nb is 0.5%, 0.15% for Ti and 0.95% for B, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為27.5%、Dy為4.0%、Cu為0.2%、Co為2.5%、Ga為0.5%、Nb為0.5%、Ti為0.15%和B為0.95%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material comprises the following components: Nd is 27.5%, Dy is 4.0%, Cu is 0.2%, Co is 2.5%, Ga is 0.5%, and Nb is 0.5%, 0.15% for Ti and 0.95% for B, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為28.5%、Dy為3.0%、Cu為0.1%、Co為1.0%、Ga為0.6%、Nb為0.3%和B為0.90%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material comprises the following components: Nd is 28.5%, Dy is 3.0%, Cu is 0.1%, Co is 1.0%, Ga is 0.6%, and Nb is 0.3% and B are 0.90%, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為27.5%、Dy為4.0%、Cu為0.15%、Co為1.0%、Ga為0.5%、Nb為0.35%、Ti為0.15%和B為0.90%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material contains the following components: Nd is 27.5%, Dy is 4.0%, Cu is 0.15%, Co is 1.0%, Ga is 0.5%, and Nb is 0.35%, 0.15% for Ti and 0.90% for B, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為26.0%、Dy為5.5%、Cu為0.2%、Co為2.0%、Ga為0.3%、Nb為0.4%、Ti為0.2%和B為0.95%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material contains the following components: Nd is 26.0%, Dy is 5.5%, Cu is 0.2%, Co is 2.0%, Ga is 0.3%, and Nb is 0.4%, 0.2% for Ti and 0.95% for B, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為25.5%、Dy為6.0%、Cu為0.3%、Co為4.0%、Ga為0.15%、Nb為0.5%、Ti為0.3%和B為1.02%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material comprises the following components: Nd is 25.5%, Dy is 6.0%, Cu is 0.3%, Co is 4.0%, Ga is 0.15%, Nb is 0.5%, Ti is 0.3%, and B is 1.02%, the balance is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the neodymium iron boron permanent magnet material.
本發明提供了一種釹鐵硼永磁材料的原料組合物,其包含下述組分:Nd為24.0~29.0%、RH為3.0~6.0%、Cu為0.1~0.3%、Co為1.0~4.0%、Ga為0.1~0.6%、Nb 為0.3~0.5%、Ti為0.0~0.3%和B為0.90~1.02%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比;所述RH為重稀土元素。The present invention provides a raw material composition of neodymium iron boron permanent magnet material, which contains the following components: Nd is 24.0-29.0%, RH is 3.0-6.0%, Cu is 0.1-0.3%, and Co is 1.0-4.0% , Ga is 0.1~0.6%, Nb is 0.3~0.5%, Ti is 0.0~0.3% and B is 0.90~1.02%, the balance is Fe and unavoidable impurities, the percentage refers to the said neodymium iron boron permanent magnet The mass percentage in the raw material composition of the material; the RH is a heavy rare earth element.
本發明中,所述Nd的含量優選為25.5~28.5%或25.5~27.5%,例如25.5%、26.0%、27.5%或28.5%,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In the present invention, the Nd content is preferably 25.5-28.5% or 25.5-27.5%, such as 25.5%, 26.0%, 27.5% or 28.5%, and the percentage refers to the raw material composition of the neodymium iron boron permanent magnet material. The mass percentage in.
本發明中,所述RH可為本領域常規的重稀土元素,例如Dy和/或Tb,優選為Dy。In the present invention, the RH may be a heavy rare earth element conventional in the art, such as Dy and/or Tb, preferably Dy.
本發明中,所述RH的含量優選為4.0~6.0%或4.0~5.5%,例如4.0%、5.5%或6.0%,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In the present invention, the RH content is preferably 4.0~6.0% or 4.0~5.5%, such as 4.0%, 5.5% or 6.0%, and the percentage refers to the mass in the raw material composition of the neodymium iron boron permanent magnet material percentage.
本發明中,所述Cu的含量優選為0.1~0.2%,例如0.1%、0.15%或0.2%,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In the present invention, the Cu content is preferably 0.1% to 0.2%, such as 0.1%, 0.15% or 0.2%, and the percentage refers to the mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
本發明中,所述Co的含量優選為1.0~3.0%或1.0~2.0%,例如1.0%、2.0%或2.5%,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In the present invention, the content of Co is preferably 1.0~3.0% or 1.0~2.0%, such as 1.0%, 2.0% or 2.5%, and the percentage refers to the mass in the raw material composition of the neodymium iron boron permanent magnet material. percentage.
本發明中,所述Ga的含量優選為0.15~0.6%或0.15~0.5%,例如0.15%、0.2%、0.3%、0.35%、0.45%、0.5%或0.6%,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In the present invention, the content of Ga is preferably 0.15~0.6% or 0.15~0.5%, such as 0.15%, 0.2%, 0.3%, 0.35%, 0.45%, 0.5% or 0.6%, and the percentage refers to the content of the neodymium The mass percentage in the raw material composition of the iron-boron permanent magnet material.
本發明中,所述Nb的含量優選為0.3~0.4%或0.3~0.35%,例如0.3%、0.35%或0.4%,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In the present invention, the Nb content is preferably 0.3 to 0.4% or 0.3 to 0.35%, such as 0.3%, 0.35% or 0.4%, and the percentage refers to the mass in the raw material composition of the neodymium iron boron permanent magnet material percentage.
本發明中,所述Ti的含量優選為0.1~0.3%或0.1~0.2%,例如0.15%、0.2%或0.3%,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In the present invention, the content of Ti is preferably 0.1 to 0.3% or 0.1 to 0.2%, such as 0.15%, 0.2% or 0.3%, and the percentage refers to the mass in the raw material composition of the neodymium iron boron permanent magnet material percentage.
本發明中,所述B的含量優選為0.92~1.02%,例如0.95%,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In the present invention, the content of B is preferably 0.92 to 1.02%, such as 0.95%, and the percentage refers to the mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
本發明中,優選地,所述Ga的含量為0.15~0.6%,所述Nb的含量為0.3~0.4%;更優選地,所述Ga的含量為0.15~0.5%,所述Nb的含量為0.3~0.35%;例如,Ga為0.20%、Nb為0.3%,Ga為0.35%、Nb為0.4%,Ga為0.45%,Nb為0.5%,Ga為0.5%、Nb為0.5%,Ga為0.6%、Nb為0.3%,Ga為0.5%、Nb為0.35%、Ga為0.3% 、Nb為0.4%,或者,Ga為0.15%、Nb為0.5%;百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In the present invention, preferably, the content of Ga is 0.15 to 0.6%, and the content of Nb is 0.3 to 0.4%; more preferably, the content of Ga is 0.15 to 0.5%, and the content of Nb is 0.3~0.35%; For example, Ga is 0.20%, Nb is 0.3%, Ga is 0.35%, Nb is 0.4%, Ga is 0.45%, Nb is 0.5%, Ga is 0.5%, Nb is 0.5%, Ga is 0.6 %, Nb is 0.3%, Ga is 0.5%, Nb is 0.35%, Ga is 0.3%, Nb is 0.4%, or Ga is 0.15%, Nb is 0.5%; the percentage refers to the neodymium iron boron permanent magnet The mass percentage of the raw material composition of the material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料的原料組合物中包含下述組分:Nd為25.5~28.5%、Dy為4.0~6.0%、Cu為0.1~0.2%、Co為1.0~3.0%、Ga為0.15~0.6%、 Nb為0.3~0.4%、Ti為0.1~0.3%和B為0.92~1.02%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron permanent magnet material contains the following components: Nd is 25.5-28.5%, Dy is 4.0-6.0%, Cu is 0.1-0.2%, Co 1.0~3.0%, Ga is 0.15~0.6%, Nb is 0.3~0.4%, Ti is 0.1~0.3% and B is 0.92~1.02%, the balance is Fe and unavoidable impurities, the percentage refers to the The mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料的原料組合物中包含下述組分:Nd為25.5~27.5%、Dy為4.0~5.5%、Cu為0.1~0.2%、Co為1.0~2.0%、Ga為0.15~0.5%、 Nb為0.3~0.35%、Ti為0.1~0.2%和B為0.92~1.02%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In a preferred embodiment of the present invention, the raw material composition of the neodymium iron boron permanent magnet material contains the following components: Nd is 25.5~27.5%, Dy is 4.0~5.5%, Cu is 0.1~0.2%, Co 1.0~2.0%, Ga is 0.15~0.5%, Nb is 0.3~0.35%, Ti is 0.1~0.2% and B is 0.92~1.02%, the balance is Fe and unavoidable impurities, the percentage refers to The mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為27.5%、Dy為4.0%、Cu為0.2%、Co為2.5%、Ga為0.20%、Nb為0.3%、Ti為0.15%和B為0.95%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material comprises the following components: Nd is 27.5%, Dy is 4.0%, Cu is 0.2%, Co is 2.5%, Ga is 0.20%, and Nb is 0.3%, 0.15% for Ti, and 0.95% for B, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為27.5%、Dy為4.0%、Cu為0.2%、Co為2.5%、Ga為0.35%、Nb為0.4%、Ti為0.15%和B為0.95%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material comprises the following components: Nd is 27.5%, Dy is 4.0%, Cu is 0.2%, Co is 2.5%, Ga is 0.35%, and Nb is 0.4%, Ti is 0.15%, and B is 0.95%, the balance is Fe and inevitable impurities, and the percentage refers to the mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為27.5%、Dy為4.0%、Cu為0.2%、Co為2.5%、Ga為0.45%、Nb為0.5%、Ti為0.15%和B為0.95%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material contains the following components: Nd is 27.5%, Dy is 4.0%, Cu is 0.2%, Co is 2.5%, Ga is 0.45%, and Nb is 0.5%, 0.15% for Ti, and 0.95% for B, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為27.5%、Dy為4.0%、Cu為0.2%、Co為2.5%、Ga為0.5%、Nb為0.5%、Ti為0.15%和B為0.95%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material comprises the following components: Nd is 27.5%, Dy is 4.0%, Cu is 0.2%, Co is 2.5%, Ga is 0.5%, and Nb is 0.5%, 0.15% for Ti, and 0.95% for B, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為28.5%、Dy為3.0%、Cu為0.1%、Co為1.0%、Ga為0.6%、Nb為0.3%和B為0.90%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material comprises the following components: Nd is 28.5%, Dy is 3.0%, Cu is 0.1%, Co is 1.0%, Ga is 0.6%, and Nb is 0.3% and B are 0.90%, the balance is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為27.5%、Dy為4.0%、Cu為0.15%、Co為1.0%、Ga為0.5%、Nb為0.35%、Ti為0.15%和B為0.90%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material contains the following components: Nd is 27.5%, Dy is 4.0%, Cu is 0.15%, Co is 1.0%, Ga is 0.5%, and Nb is 0.35%, 0.15% for Ti and 0.90% for B, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為26.0%、Dy為5.5%、Cu為0.2%、Co為2.0%、Ga為0.3%、Nb為0.4%、Ti為0.2%和B為0.95%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material contains the following components: Nd is 26.0%, Dy is 5.5%, Cu is 0.2%, Co is 2.0%, Ga is 0.3%, and Nb is 0.4%, 0.2% for Ti, and 0.95% for B, the remainder is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
在本發明一優選實施方式中,所述釹鐵硼永磁材料包含下述組分:Nd為25.5%、Dy為6.0%、Cu為0.3%、Co為4.0%、Ga為0.15%、Nb為0.5%、Ti為0.3%和B為1.02%,餘量為Fe及不可避免的雜質,百分比是指在所述釹鐵硼永磁材料的原料組合物中的質量百分比。In a preferred embodiment of the present invention, the neodymium iron boron permanent magnet material comprises the following components: Nd is 25.5%, Dy is 6.0%, Cu is 0.3%, Co is 4.0%, Ga is 0.15%, Nb is 0.5%, Ti is 0.3%, and B is 1.02%, the balance is Fe and unavoidable impurities, and the percentage refers to the mass percentage in the raw material composition of the neodymium iron boron permanent magnet material.
本發明還提供了一種釹鐵硼永磁材料的製備方法,其包括下述步驟:將所述的釹鐵硼永磁材料的原料組合物經熔煉澆鑄、破碎、成型和燒結處理,即可。The present invention also provides a method for preparing a neodymium iron boron permanent magnet material, which includes the following steps: the raw material composition of the neodymium iron boron permanent magnet material is smelted and cast, crushed, shaped and sintered.
本發明中,所述熔煉澆鑄的工藝可為本領域常規的熔煉澆鑄工藝,例如在中頻真空熔煉爐中進行熔煉澆鑄。In the present invention, the smelting and casting process can be a conventional smelting and casting process in the field, for example, smelting and casting are performed in an intermediate frequency vacuum melting furnace.
其中,所述中頻真空熔煉爐可為中頻真空感應速凝甩帶爐。在所述中頻真空感應速凝甩帶爐經熔煉澆鑄工藝製得的甩片厚度一般為0.2~0.4mm,優選為0.26~0.29mm。 所述中頻的頻率可為1500~2500Hz。Wherein, the intermediate frequency vacuum smelting furnace may be an intermediate frequency vacuum induction rapid solidification belt spinning furnace. The thickness of the spun sheet produced by the smelting and casting process in the intermediate frequency vacuum induction quick-setting belt spinning furnace is generally 0.2 to 0.4 mm, preferably 0.26 to 0.29 mm. The frequency of the intermediate frequency may be 1500~2500 Hz.
本發明中,所述破碎的工藝可為本領域常規的破碎工藝,例如經吸氫處理、脫氫處理,即可。In the present invention, the crushing process can be a conventional crushing process in the field, such as hydrogen absorption treatment and dehydrogenation treatment.
其中,所述吸氫處理和/或所述脫氫處理可在氫破爐中進行。Wherein, the hydrogen absorption treatment and/or the dehydrogenation treatment can be carried out in a hydrogen furnace.
其中,所述吸氫處理可在氫氣壓力0.1~0.15MPa的條件下進行。當氫破壓力變化範圍小於0.04MPa/10min時,可認為吸氫處理完成。Wherein, the hydrogen absorption treatment can be carried out under the condition of a hydrogen pressure of 0.1 to 0.15 MPa. When the hydrogen breaking pressure change range is less than 0.04MPa/10min, it can be considered that the hydrogen absorption treatment is completed.
其中,所述脫氫處理可在500~600°C保溫條件下進行,例如550°C。 所述保溫的時間可為2~4h,例如4h。Wherein, the dehydrogenation treatment can be carried out under the temperature of 500-600°C, for example, 550°C. The heat preservation time may be 2 to 4 hours, for example, 4 hours.
其中,所述脫氫處理後,粉體的氫含量一般可為500~2000ppm。Wherein, after the dehydrogenation treatment, the hydrogen content of the powder may generally be 500 to 2000 ppm.
本發明中,所述破碎後,還可按本領域常規手段進行粉碎處理,例如經氣流磨粉碎。In the present invention, after the crushing, the crushing treatment can be carried out according to conventional means in the field, for example, crushing by jet mill.
其中,所述氣流磨粉碎之前,還可添加抗氧化劑和/或潤滑劑。所述抗氧化劑和所述潤滑劑一般不應與所述釹鐵硼永磁材料中的原料發生化學反應。Wherein, before the jet mill is pulverized, an antioxidant and/or a lubricant may be added. The antioxidant and the lubricant generally should not chemically react with the raw materials in the neodymium iron boron permanent magnet material.
所述抗氧化劑和/或所述潤滑劑的添加,一則能夠防止粉料在磨粉過程中發生氧化;二則減少粉體的摩擦係數,易於成型。The addition of the antioxidant and/or the lubricant can prevent the powder from being oxidized during the grinding process; secondly, it can reduce the friction coefficient of the powder and facilitate molding.
其中,所述氣流磨粉碎過程中,粉碎氣氛中的氧含量優選為40~60ppm。Wherein, during the jet mill pulverization process, the oxygen content in the pulverizing atmosphere is preferably 40-60 ppm.
當所述粉碎氣氛中的氧含量<40ppm時,後續成型和燒結拆袋等工藝管控難度較大,釹鐵硼永磁材料易發生不均勻的氧化。When the oxygen content in the pulverizing atmosphere is less than 40 ppm, it is difficult to control the subsequent forming, sintering, and bag removal processes, and the neodymium iron boron permanent magnet material is prone to uneven oxidation.
當所述粉碎氣氛中的氧含量>60ppm時,可能會降低釹鐵硼永磁材料的剩磁和矯頑力,若在氣流磨階段發生部分氧化,有可能導致燒結難以成型。When the oxygen content in the pulverizing atmosphere is greater than 60 ppm, the remanence and coercivity of the neodymium iron boron permanent magnet material may be reduced. If partial oxidation occurs during the jet milling stage, it may cause sintering and forming difficult.
其中,所述氣流磨粉碎後,所述釹鐵硼永磁材料的粒徑可為D50為3.4~3.7μm,例如D50為3.5μm。Wherein, after the jet mill pulverization, the particle size of the neodymium iron boron permanent magnet material can be D50 of 3.4-3.7 μm, for example, D50 of 3.5 μm.
本發明中,所述成型的工藝可為本領域常規的成型工藝,例如磁場取向壓制成型或熱壓熱變型。In the present invention, the molding process can be a conventional molding process in the field, such as magnetic field orientation compression molding or hot pressing and thermal deformation.
其中,所述磁場取向壓制成型可在惰性氣體氣氛中進行。所述惰性氣體可為本領域常規的惰性氣體,例如氮氣或氬氣。Wherein, the magnetic field orientation compression molding can be performed in an inert gas atmosphere. The inert gas may be a conventional inert gas in the art, such as nitrogen or argon.
其中,所述磁場取向壓制成型後,還可在壓力>240MPa的條件下進行冷等靜壓處理。Wherein, after the magnetic field orientation compression molding, cold isostatic pressing treatment can also be performed under the condition of pressure> 240 MPa.
本發明中,所述燒結處理優選在惰性氣體氣氛中進行;更優選地,所述燒結處理的工藝按下述步驟進行,在惰性氣體氣氛中,經燒結和冷卻,即可。In the present invention, the sintering treatment is preferably carried out in an inert gas atmosphere; more preferably, the sintering treatment process is carried out according to the following steps, in an inert gas atmosphere, sintering and cooling are required.
其中,所述燒結過程中的惰性氣體可為本領域常規的惰性氣體,優選為氬氣或氦氣。所述惰性氣體一般不應與所述釹鐵硼永磁材料發生化學反應。Wherein, the inert gas in the sintering process can be a conventional inert gas in the art, preferably argon or helium. The inert gas generally should not chemically react with the neodymium iron boron permanent magnet material.
其中,優選地,所述燒結在-0.05MPa的惰性氣體氣氛中進行,例如-0.05MPa的氬氣氣氛中。Among them, preferably, the sintering is performed in an inert gas atmosphere of -0.05 MPa, for example, in an argon atmosphere of -0.05 MPa.
其中,所述燒結可在燒結爐中進行。一般而言,經所述成型處理後獲得的壓坯可置於真空燒結爐中。優選地,所述燒結爐在通入所述惰性氣體之前,還經放氣處理。所述放氣處理可在800~900°C的條件下進行,例如860°C。Wherein, the sintering can be performed in a sintering furnace. Generally speaking, the compact obtained after the forming process can be placed in a vacuum sintering furnace. Preferably, the sintering furnace is also subjected to a gas release treatment before the inert gas is introduced. The outgassing treatment can be performed at 800 to 900°C, for example, 860°C.
當所述燒結處理在惰性氣體氣氛中進行時,相比於真空燒結,能夠有效減少稀土元素的揮發,增加爐內加熱傳熱速率和均溫區。When the sintering process is performed in an inert gas atmosphere, compared to vacuum sintering, the volatilization of rare earth elements can be effectively reduced, and the heating heat transfer rate and the uniform temperature zone in the furnace can be increased.
其中,所述燒結的溫度可為本領域常規的燒結溫度,例如1050~1090°C,再例如1080°C。Wherein, the sintering temperature may be a conventional sintering temperature in the art, for example, 1050-1090°C, and for example, 1080°C.
其中,所述燒結的時間可為本領域常規的燒結時間,例如4~8h,再例如5h。Wherein, the sintering time may be a conventional sintering time in the art, for example, 4-8h, and for example 5h.
其中,所述冷卻的工藝可為本領域常規的冷卻工藝,例如開風機快速風冷至60°C以下,即可。Wherein, the cooling process can be a conventional cooling process in the field, for example, a fan can be used for rapid air cooling to below 60°C.
其中,所述冷卻後還可按本領域常規的工藝進行時效處理。所述時效處理可分為一級時效處理和二級時效處理。所述一級時效處理可在900°C 條件下進行。所述二級時效處理可在630°C條件下進行。Wherein, after the cooling, an aging treatment can be performed according to a conventional process in the field. The aging treatment can be divided into primary aging treatment and secondary aging treatment. The primary aging treatment can be carried out at 900°C. The secondary aging treatment can be carried out at 630°C.
本發明還提供了一種採用前述方法製得的釹鐵硼永磁材料。The invention also provides a neodymium iron boron permanent magnet material prepared by the aforementioned method.
其中,所述釹鐵硼永磁材料中的氧含量優選為1000~1300ppm。Wherein, the oxygen content in the neodymium iron boron permanent magnet material is preferably 1000 to 1300 ppm.
本發明還提供了一種所述的釹鐵硼永磁材料在電機中作為電子元器件的應用。The invention also provides an application of the neodymium iron boron permanent magnet material as an electronic component in a motor.
其中,所述電機優選為用於交通運輸領域的稀土永磁電機和/或用於電子產品的電機。Wherein, the motor is preferably a rare earth permanent magnet motor used in the field of transportation and/or a motor used in electronic products.
所述用於交通運輸領域的稀土永磁電機可為電動車中的驅動器電機和/或電動汽車中的車輛牽引電機。The rare earth permanent magnet motor used in the transportation field may be a driver motor in an electric vehicle and/or a vehicle traction motor in an electric vehicle.
所述電子產品可為計算機、手機震動電機和電聲揚聲器中的一種或多種。The electronic product may be one or more of a computer, a vibration motor of a mobile phone, and an electro-acoustic speaker.
在符合本領域常識的基礎上,上述各優選條件,可任意組合,即得本發明各較佳實例。On the basis of conforming to common knowledge in the field, the above-mentioned preferred conditions can be combined arbitrarily to obtain preferred examples of the present invention.
本發明所用試劑和原料均市售可得。The reagents and raw materials used in the present invention are all commercially available.
本發明的積極進步效果在於:The positive and progressive effects of the present invention are:
本發明通過在配方中添加含量≧0.3 wt.%的Nb,同時添加能夠富集在晶界阻止晶粒的異常長大和增加晶界相的元素Ga,Nb和Ga和在晶界相中形成能阻礙晶粒長大的含Nb的化合物,Br≧1.29 T、Hcj≧1933 kA/m的條件下,獲得了在20~100°C溫度區間磁通溫度係數α的絕對值≦0.085%/°C的釹鐵硼永磁材料。In the present invention, by adding Nb with a content of ≧0.3 wt.% to the formula, and at the same time adding elements Ga, Nb and Ga that can be enriched at the grain boundary to prevent the abnormal growth of grains and increase the grain boundary phase, and the formation energy in the grain boundary phase Nb-containing compounds that hinder the growth of crystal grains, under the conditions of Br≧1.29 T and Hcj≧1933 kA/m, the absolute value of the magnetic flux temperature coefficient α in the temperature range of 20~100°C is obtained ≦0.085%/°C NdFeB permanent magnet material.
下面通過實施例的方式進一步說明本發明,但並不因此將本發明限制在所述的實施例範圍之中。下列實施例中未註明具體條件的實驗方法,按照常規方法和條件,或按照商品說明書選擇。The present invention will be further described by way of examples below, but the present invention is not limited to the scope of the described examples. The experimental methods without specific conditions in the following examples are selected in accordance with conventional methods and conditions, or in accordance with the product specification.
下述實施例及對比例中,防氧化劑及潤滑劑購自天津悅聖新材料研究所生產的釹鐵硼防氧化劑和潤滑劑。In the following examples and comparative examples, the antioxidants and lubricants were purchased from the neodymium iron boron antioxidants and lubricants produced by Tianjin Yuesheng New Materials Research Institute.
實施例及對比例中燒結釹鐵硼磁鐵的配方如表1所示。表1中wt.%是指組分在釹鐵硼永磁材料的原料組合物中的質量百分比,"/"表示未添加該元素。The formulations of the sintered NdFeB magnets in the examples and comparative examples are shown in Table 1. The wt.% in Table 1 refers to the mass percentage of the component in the raw material composition of the neodymium iron boron permanent magnet material, and "/" means that the element is not added.
表1 Table 1
燒結釹鐵硼的製備方法:The preparation method of sintered NdFeB:
(1)按照表1所示的原料比例進行配料,並將配方的原材料放入中頻真空熔煉爐(中頻真空感應速凝甩帶爐)中進行熔煉、澆鑄。製備的甩片平均厚度0.26~0.29mm之間,並經自動選片機剔除甩片厚度不在0.2~0.4mm之間的厚片和薄片;(1) Prepare ingredients according to the ratio of raw materials shown in Table 1, and put the raw materials of the formula into an intermediate frequency vacuum melting furnace (medium frequency vacuum induction quick-setting belt spinning furnace) for smelting and casting. The average thickness of the prepared splinters is between 0.26~0.29mm, and the thick slices and flakes with the splinter thickness not between 0.2~0.4mm are rejected by the automatic selection machine;
(2)在氫破爐中飽和吸氫至氫氣壓力不再變化(通入氫氣壓力約0.1~0.15MPa,等到氫破壓力變化範圍小於0.04MPa/10min時,認為完成吸氫階段),並在550°C溫度下保溫4h脫氫,粉體處在半脫氫狀態(脫氫後粉體的氫含量為500~2000ppm);在粉體中添加燒結釹鐵硼專用的防氧化劑及潤滑劑,在氧含量為40~60ppm的條件下,在氣流磨中製備出粉體粒度D50=3.5μm;(2) Saturate and absorb hydrogen in the hydrogen breaker until the hydrogen pressure does not change (the pressure of the hydrogen is about 0.1~0.15MPa. When the change range of the hydrogen breakage pressure is less than 0.04MPa/10min, the hydrogen absorption stage is considered to be completed), and Dehydrogenation at a temperature of 550°C for 4 hours, the powder is in a semi-dehydrogenated state (the hydrogen content of the powder after dehydrogenation is 500~2000ppm); add sintered NdFeB special antioxidant and lubricant to the powder, Under the condition that the oxygen content is 40~60ppm, the powder particle size D50=3.5μm is prepared in the jet mill;
(3)在壓機磁場取向下壓制成型,並經壓力>240MPa的冷等靜壓處理。在氮氣含量低於100ppm的環境下拆袋進入到真空燒結爐中。在860°C放氣階段結束後,通入燒結爐內壓力為-0.05MPa的氬氣,以減少燒結爐內壓力差和減少稀土元素的揮發,從而增加爐內加熱傳熱速率和均溫區。在1080°C燒結5個小時後,風冷至60°C以下出爐,並分別進行900°C一級時效和630°C二級時效。然後製出D10*10mm的樣品。(3) Compression molding is performed under the orientation of the magnetic field of the press, and subjected to cold isostatic pressing with a pressure> 240 MPa. In an environment where the nitrogen content is less than 100ppm, the bag is removed and entered into the vacuum sintering furnace. After the degassing stage at 860°C, argon gas with a pressure of -0.05MPa is introduced into the sintering furnace to reduce the pressure difference in the sintering furnace and reduce the volatilization of rare earth elements, thereby increasing the heating heat transfer rate and uniform temperature zone in the furnace . After sintering at 1080°C for 5 hours, it is air-cooled to below 60°C and out of the furnace, and the first-stage aging at 900°C and the second-stage aging at 630°C are performed respectively. Then make a D10*10mm sample.
效果實施例Example of effects
使用中國計量院的NIM-10000H型BH大塊稀土永磁無損測量系統,對實施例1-8、對比例1-12製得的燒結釹鐵磁硼鐵進行磁性能檢測。下表2所示為磁性能檢測結果。表2中,"Br"為殘留磁通密度(remanence),"Hcj"為內稟矯頑力,"Hk/Hcj"為角形比(squareness ratio)。The NIM-10000H type BH bulk rare earth permanent magnet non-destructive measurement system of the China Metrology Institute was used to test the magnetic properties of the sintered NdFeB magnets prepared in Examples 1-8 and Comparative Examples 1-12. Table 2 below shows the magnetic performance test results. In Table 2, "Br" is the remanence, "Hcj" is the intrinsic coercivity, and "Hk/Hcj" is the squareness ratio.
氧含量採用氧氮氫分析儀進行檢測。The oxygen content is detected by an oxygen, nitrogen and hydrogen analyzer.
表2 Table 2
由表2可知:It can be seen from Table 2:
(1)本申請中的釹鐵硼永磁材料性能優異,Br≧1.29 T、Hcj≧1933 kA/m、磁通溫度係數α的絕對值≦0.085%/°C,在保持釹鐵硼永磁材料的Hcj和Br的基礎上,降低了磁通溫度係數(實施例1-8);(1) The NdFeB permanent magnet material in this application has excellent performance, Br≧1.29 T, Hcj≧1933 kA/m, and the absolute value of the magnetic flux temperature coefficient α≦0.085%/°C, while maintaining the NdFeB permanent magnet Based on the Hcj and Br of the material, the temperature coefficient of magnetic flux is reduced (Examples 1-8);
(2)基於本申請的配方,原料Ga、Nb、Cu和Co的用量改變,釹鐵硼永磁材料的性能明顯下降(對比例1-9);(2) Based on the formula of this application, the amount of raw materials Ga, Nb, Cu and Co is changed, and the performance of the neodymium iron boron permanent magnet material is significantly reduced (Comparative Examples 1-9);
(3)基於本申請的配方,將Ga替換為性能相似的Al,或是將Nb替換為性能相似的Zr,或是將Co替換為性能相似的Mn,均無法獲得本申請中的磁通溫度係數的釹鐵硼永磁材料(對比例10-13)。(3) Based on the formula of this application, replacing Ga with Al with similar properties, or replacing Nb with Zr with similar properties, or replacing Co with Mn with similar properties, will not be able to obtain the magnetic flux temperature in this application. Coefficient of neodymium iron boron permanent magnet material (comparative examples 10-13).
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