CN102528052A - Preparation method for quickly quenched Fe-based metal grain with excellent wave absorbing property - Google Patents

Preparation method for quickly quenched Fe-based metal grain with excellent wave absorbing property Download PDF

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CN102528052A
CN102528052A CN2011104408270A CN201110440827A CN102528052A CN 102528052 A CN102528052 A CN 102528052A CN 2011104408270 A CN2011104408270 A CN 2011104408270A CN 201110440827 A CN201110440827 A CN 201110440827A CN 102528052 A CN102528052 A CN 102528052A
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谢国治
宦峰
郭稷
宋晓龙
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Hohai University HHU
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Abstract

本发明提供了一种用超声波制备具有吸波特性的快淬Fe-基金属颗粒的方法。将各金属元素在合金中所占的质量百分比称取相应的金属配成磁性金属合金,并在熔炼、甩带、球磨后通过超声波分散处理得到的能够改善界面特性与分布均匀的具有优良吸波特性的Fe-基金属颗粒材料。本发明从利用超声波在液体中的空化原理和机械效应出发来获得快淬Fe-基金属颗粒分散均匀的材料,同时超声波在压电材料和磁致伸缩材料中传播时,由于超声波的机械作用而引起的感生电极化和感生磁化,从而提高Fe-基金属颗粒材料的吸波特性。本发明原理正确,手段科学,用本发明获得的一种具有良好吸波特性的块淬Fe-基金属颗粒材料,有很高的实用价值,广泛的应用前景。The invention provides a method for preparing fast-quenching Fe-based metal particles with wave-absorbing characteristics by using ultrasonic waves. The mass percentage of each metal element in the alloy is weighed and the corresponding metal is made into a magnetic metal alloy, and after smelting, stripping, and ball milling, it is obtained through ultrasonic dispersion treatment, which can improve the interface characteristics and distribute uniformly. Characteristics of Fe-based metal particulate materials. The present invention starts from the cavitation principle and mechanical effect of ultrasonic waves in liquids to obtain materials with uniform dispersion of rapidly quenched Fe-based metal particles. At the same time, when ultrasonic waves propagate in piezoelectric materials and magnetostrictive materials, due to the mechanical action of ultrasonic waves The induced electric polarization and induced magnetization are induced, thereby improving the wave-absorbing characteristics of the Fe-based metal particle material. The principle of the invention is correct, and the method is scientific. The bulk quenched Fe-based metal particle material with good wave-absorbing properties obtained by the invention has high practical value and wide application prospect.

Description

一种具有良好吸波特性的快淬Fe-基金属颗粒的制备方法A Preparation Method of Rapidly Quenched Fe-Based Metal Particles with Good Wave Absorbing Properties

技术领域 technical field

本发明涉及一种具有吸波特性的金属颗粒材料,特别是具有良好吸波特性的快淬Fe-基金属颗粒材料的制备方法。  The invention relates to a metal particle material with wave-absorbing properties, especially a method for preparing a fast-quenched Fe-based metal particle material with good wave-absorbing properties. the

背景技术 Background technique

随着现代科学技术的发展,电磁波辐射对环境的影响日益增大。在机场,飞机航班因电磁波干扰无法起飞而误点;在医院,移动电话常会干扰各种电子诊疗仪器的正常工作;在日益重要的隐身和电磁兼容(EMC)技术中,电磁波吸收材料的作用和地位也显得十分突出,已成为现代军事中电子对抗的法宝和“秘密武器”。因此,治理电磁污染,寻找一种具有优良吸波特性的材料,已成为材料科学的一大课题。  With the development of modern science and technology, the impact of electromagnetic radiation on the environment is increasing. At airports, airplane flights are delayed due to electromagnetic wave interference; in hospitals, mobile phones often interfere with the normal work of various electronic medical instruments; in increasingly important stealth and electromagnetic compatibility (EMC) technologies, the role and status of electromagnetic wave absorbing materials It also appears very prominent, and has become a magic weapon and "secret weapon" for electronic countermeasures in modern military affairs. Therefore, controlling electromagnetic pollution and finding a material with excellent wave-absorbing properties have become a major topic in material science. the

吸波材料研究不仅在军事上有着重大意义,而且对民用电子行业如抗干扰器件的开发也起着推动作用。寻找具有优良吸波特性材料的新设计方法一直是人们寻求的目的,但吸波材料存在着对电磁波的反射问题。虽然到目前为止人们已经研究了不少的电磁波吸收材料,但仍无法做到无反射吸收,只能尽可能高的提高材料的吸波特性,因此距离实际应用仍旧有不小的距离。  Research on absorbing materials is not only of great significance in the military, but also plays a role in promoting the development of civilian electronics such as anti-jamming devices. Finding a new design method for materials with excellent wave-absorbing properties has always been the purpose of people's pursuit, but there is a problem of reflection of electromagnetic waves in wave-absorbing materials. Although people have studied a lot of electromagnetic wave absorbing materials so far, they still cannot achieve non-reflective absorption. They can only improve the wave-absorbing characteristics of materials as high as possible, so there is still a long way to go for practical applications. the

发明内容 Contents of the invention

本发明的目的在于提供一种制备具有良好吸波特性的快淬Fe-基金属颗粒材料的方法,这种具有良好吸波特性的快淬Fe-基金属颗粒材料的制备方法其特征是使用以下步骤:  The object of the present invention is to provide a kind of method that prepares the fast-quenching Fe-based metal particle material with good wave-absorbing characteristic, the preparation method of this fast-quenching Fe-base metal particle material with good wave-absorbing characteristic is characterized in that Use the following steps:

(1)Fe-基金属合金的制备:将高纯铁棒(99.9wt%)比例为65-70%、钕块(99.9wt%)比例为2-4%、分析纯钴片(99.8wt%)比例为16-20%、分析纯硼(99.8wt%)比例为9-13%,按各元素在合金中所占的原子百分比 称取相应质量的金属,配成磁性金属合金,放入高频感应熔炼炉内熔炼得到合金铸锭;  (1) Preparation of Fe-based metal alloy: the proportion of high-purity iron rod (99.9wt%) is 65-70%, the proportion of neodymium block (99.9wt%) is 2-4%, and the proportion of analytical pure cobalt sheet (99.8wt%) 16-20%, and the proportion of analytically pure boron (99.8wt%) is 9-13%. According to the atomic percentage of each element in the alloy, the corresponding mass of metal is weighed, made into a magnetic metal alloy, and placed in a high-frequency induction Alloy ingots are obtained by smelting in a smelting furnace;

(2)Fe-基金属薄带的制备:将(1)中所得的磁性金属合金采用真空快淬炉熔炼甩带,将合金铸锭放入坩埚,抽真空后充氩至0.05MP,在钼轮外沿线速度为20-40m/s的状态下,由钨铈电极高压电弧后将合金铸锭熔化,由高速旋转的钼轮将熔化了的溶液甩成薄带;  (2) Preparation of Fe-based metal thin strip: the magnetic metal alloy obtained in (1) is smelted in a vacuum quenching furnace and thrown away, the alloy ingot is put into a crucible, and the argon is filled to 0.05MP after vacuuming, and the molybdenum When the speed along the outer wheel is 20-40m/s, the alloy ingot is melted by the tungsten-cerium electrode after the high-voltage arc, and the molten solution is thrown into a thin strip by the high-speed rotating molybdenum wheel;

(3)Fe-基金属颗粒的制备:将(2)中所得的薄带先用粉碎机粗碎,再用行星球磨机加入无水乙醇细磨,球料比10∶1,转速500r/min,每20min反转一次,球磨时间为2h,将球磨2h后的磨料阴干;  (3) Preparation of Fe-based metal particles: the thin strip obtained in (2) is first coarsely crushed with a pulverizer, and then finely ground by adding absolute ethanol with a planetary ball mill, the ball-to-material ratio is 10:1, and the rotating speed is 500r/min. Reverse once every 20 minutes, the ball milling time is 2 hours, and the abrasive after ball milling for 2 hours is dried in the shade;

(4)将(3)中所得的磨料放入烧杯中并加入适量无水乙醇,用玻璃棒充分搅拌均匀后,放入超声波设备水槽的正中央,其中水槽中的水高于烧杯中粉末高度;开启超声波设备,并设置超声频率2.5-3.5GHz,对磨料进行超声处理20-40min;  (4) Put the abrasive obtained in (3) into a beaker and add an appropriate amount of absolute ethanol. After stirring well with a glass rod, put it into the center of the water tank of the ultrasonic equipment, where the water in the water tank is higher than the powder in the beaker. ;Turn on the ultrasonic equipment, set the ultrasonic frequency to 2.5-3.5GHz, and perform ultrasonic treatment on the abrasive for 20-40min;

(5)将(4)中所得的磨料放入烘箱烘干后过筛,得到目数为200-300目的均匀Fe-基金属粉末颗粒。  (5) Put the abrasive obtained in (4) into an oven for drying and then sieve to obtain uniform Fe-based metal powder particles with a mesh size of 200-300 mesh. the

本发明优点与效果  Advantages and effects of the present invention

将(5)中所得的Fe-基金属粉末颗粒材料做成标准测量环测其电磁参量,经过线传输理论计算反射损耗后发现:  The obtained Fe-based metal powder particle material in (5) is made into a standard measurement ring to measure its electromagnetic parameters, and after calculating the reflection loss through the line transmission theory, it is found that:

磁损耗μ″与磁导率μ′均有小幅度的降低,但降低并不明显;介电损耗ε″与介电常数ε′得到了明显降低,形成了更佳阻抗匹配条件,反射损耗得到了大幅提升,即金属颗粒材料的吸波特性有了明显提高。  Both the magnetic loss μ″ and the magnetic permeability μ′ have a small decrease, but the reduction is not obvious; the dielectric loss ε″ and the dielectric constant ε′ have been significantly reduced, forming a better impedance matching condition, and the reflection loss is obtained It has been greatly improved, that is, the wave-absorbing characteristics of metal particle materials have been significantly improved. the

与现有技术相比,本发明从利用超声波在液体中的空化原理和机械效应出发来获得快淬Fe-基金属颗粒分散均匀的材料,同时超声波在压电材料和磁致伸缩材 料中传播时,由于超声波的机械作用而引起的感生电极化和感生磁化,从而提高Fe-基金属颗粒材料的吸波特性。本发明原理正确,手段科学,用本发明获得的一种具有良好吸波特性的块淬Fe-基金属颗粒材料,有很高的实用价值,广泛的应用前景。  Compared with the prior art, the present invention proceeds from the cavitation principle and mechanical effect of ultrasonic waves in liquids to obtain materials with uniform dispersion of rapidly quenched Fe-based metal particles, while ultrasonic waves are used in piezoelectric materials and magnetostrictive materials. When propagating, due to the induced electric polarization and induced magnetization caused by the mechanical action of ultrasonic waves, the wave-absorbing characteristics of Fe-based metal particle materials are improved. The principle of the invention is correct, and the method is scientific. The bulk quenched Fe-based metal particle material with good wave-absorbing properties obtained by the invention has high practical value and wide application prospect. the

附图说明 Description of drawings

图1A为本发明实施例1中测得样品的磁损耗μ″特性图  Fig. 1A is the magnetic loss μ " characteristic figure of sample measured in embodiment 1 of the present invention

图1B为本发明实施例1中测得样品的磁导率μ′特性图  Fig. 1 B is the magnetic permeability μ ' characteristic diagram of the sample measured in embodiment 1 of the present invention

图1C为本发明实施例1中测得样品的介电损耗ε″特性图  Fig. 1 C is the dielectric loss ε " characteristic figure of sample measured in embodiment 1 of the present invention

图1D为本发明实施例1中测得样品的介电常数ε′特性图  Fig. 1 D is the dielectric constant ε ' characteristic diagram of the sample measured in Example 1 of the present invention

图1E为本发明实施例1中测得样品的反射损耗特性图  Figure 1E is a reflection loss characteristic diagram of the sample measured in Example 1 of the present invention

图2为本发明实施例2中测得样品的反射损耗特性图  Fig. 2 is the reflection loss characteristic diagram of sample measured in embodiment 2 of the present invention

图3为本发明实施例3中测得样品的反射损耗特性图  Fig. 3 is the reflection loss characteristic figure of sample measured in embodiment 3 of the present invention

具体实施方式 Detailed ways

为了更好的理解本发明,以下实施例进一步阐明本发明的内容,以下实施例旨在说明本发明而不是对本发明的进一步限定,本领域的技术人员根据上述本发明的内容做出一些非本质的改进和调整,均属于本发明保护范围。  In order to better understand the present invention, the following examples further illustrate the content of the present invention, the following examples are intended to illustrate the present invention rather than further limit the present invention, those skilled in the art make some non-essential according to the above-mentioned content of the present invention Improvements and adjustments all belong to the protection scope of the present invention. the

实施例1:  Example 1:

(1)将高纯铁棒(99.9wt%)比例为65-70%、钕块(99.9wt%)比例为2-4%、分析纯钴片(99.8wt%)比例为16-20%、分析纯硼(99.8wt%)比例为9-13%,按各元素在合金中所占的原子百分比称取相应质量的金属,配成磁性金属合金,放入高频感应熔炼炉内熔炼得到合金铸锭,为确保成分的均匀性,反复熔炼两次。  (1) The proportion of high-purity iron rod (99.9wt%) is 65-70%, the proportion of neodymium block (99.9wt%) is 2-4%, the proportion of analytical pure cobalt sheet (99.8wt%) is 16-20%, analytical pure The proportion of boron (99.8wt%) is 9-13%. Weigh the corresponding mass of metal according to the atomic percentage of each element in the alloy, make it into a magnetic metal alloy, and melt it in a high-frequency induction melting furnace to obtain an alloy ingot. , in order to ensure the uniformity of the ingredients, the melting was repeated twice. the

采用真空快淬炉熔炼甩带。将合金铸锭放入坩埚,在抽真空后充氩的状态下,由钨铈电极高压电弧后将合金铸锭熔化,由高速旋转的钼轮将熔化了的溶液甩成薄带。然后将所得带状物先用粉碎机粗碎,再用行星球磨机加入无水乙醇细磨2h后阴干。其中球料比10∶1,转速500r/min,每20min反转一次。  Melting strips are smelted in a vacuum quenching furnace. Put the alloy ingot into the crucible, under the state of vacuuming and filling with argon, the alloy ingot is melted by the high-voltage arc of the tungsten-cerium electrode, and the molten solution is thrown into a thin strip by the high-speed rotating molybdenum wheel. Then the obtained ribbons were roughly crushed with a pulverizer, then finely ground with anhydrous ethanol for 2 hours with a planetary ball mill, and then dried in the shade. Among them, the ratio of ball to material is 10:1, the speed is 500r/min, and the rotation is reversed every 20min. the

将阴干后的磨料倒入烧杯并加入适量无水乙醇后放入超声波设备的水槽中,开启超声波,设置超声频率为2.5GHz,超声时长20min。  Pour the dried abrasive into a beaker and add an appropriate amount of absolute ethanol, then put it into the water tank of the ultrasonic equipment, turn on the ultrasonic wave, set the ultrasonic frequency to 2.5 GHz, and the ultrasonic time to 20 min. the

最后将超声后的磨料放入烘箱,充分干燥后过筛,得到目数为200-300目的均匀Nd-Fe-Co-基金属粉末颗粒。  Finally, the ultrasonic abrasive is put into an oven, fully dried and sieved to obtain uniform Nd-Fe-Co-based metal powder particles with a mesh number of 200-300. the

将以上制备所得的Nd-Fe-Co基磁性金属颗粒与未作任何处理的Nd-Fe-Co基磁性金属颗粒(膜厚度1.5mm)按线传输理论经反射损耗计算并通过对比后如图1所示,发现:  The Nd-Fe-Co-based magnetic metal particles prepared above and the untreated Nd-Fe-Co-based magnetic metal particles (film thickness 1.5 mm) were calculated according to the line transmission theory and reflected by the comparison, as shown in Figure 1 As shown, found:

(1)经超声波分散处理后,磁损耗μ″有小幅度的降低,降幅低于1-2%。  (1) After ultrasonic dispersion treatment, the magnetic loss μ" has a small decrease, and the decrease rate is less than 1-2%. 

(2)经超声波分散处理后,磁导率μ′有小幅度的降低,降幅低于1-2%。  (2) After the ultrasonic dispersion treatment, the magnetic permeability μ' has a small decrease, and the decrease rate is less than 1-2%. the

(3)经超声波分散处理后,介电损耗ε″降低幅度较大,在2GHz时,介电损耗由未作处理样品的55降低到15,降幅超过50%。  (3) After ultrasonic dispersion treatment, the dielectric loss ε″ has been greatly reduced. At 2 GHz, the dielectric loss has been reduced from 55 to 15 for the untreated sample, a drop of more than 50%. 

(4)经超声波分散处理后,介电常数ε′得到了明显降低,在2GHz时,由未作处理样品的115降低到65,降幅超过40%。  (4) After ultrasonic dispersion treatment, the dielectric constant ε' has been significantly reduced. At 2GHz, it has been reduced from 115 to 65 in the untreated sample, a decrease of more than 40%. the

(5)经超声波分散处理后,反射损耗dB得到了大幅提升,未超声前的最大反射损耗值由2.2GHz的-6.5dB,而超声后的最大反射损耗在3.1GHz处达到-11.4dB,相对于未作处理的样品最大反射损耗提升了超过90%。  (5) After ultrasonic dispersion treatment, the reflection loss dB has been greatly improved. The maximum reflection loss value before ultrasound is -6.5dB at 2.2GHz, and the maximum reflection loss after ultrasound is -11.4dB at 3.1GHz, which is relatively Compared with the untreated sample, the maximum reflection loss is increased by more than 90%. the

综上所述,在经超声波分散处理后的Nd-Fe-Co基磁性金属颗粒材料得到了比未经超声波分散处理的Nd-Fe-Co基磁性金属颗粒材料具有更优良的吸波特性。  In summary, the Nd-Fe-Co-based magnetic metal particle material after ultrasonic dispersion treatment has better wave-absorbing characteristics than the Nd-Fe-Co-based magnetic metal particle material without ultrasonic dispersion treatment. the

实施例2:  Example 2:

与实施例1中的制备Nd-Fe-Co基磁性金属颗粒材料的方法相同,但将超声频率设置为3.0GHz,超声时长30min。将制备所得的Nd-Fe-Co基磁性金属颗粒与未作任何处理的Nd-Fe-Co基磁性金属颗粒(膜厚度1.5mm)按线传输理论经反射损耗计算并通过对比后(见图2)得到了与实施例1相一致的结论。  The method for preparing the Nd-Fe-Co-based magnetic metal particle material in Example 1 is the same, but the ultrasonic frequency is set to 3.0 GHz, and the ultrasonic time is 30 min. The prepared Nd-Fe-Co-based magnetic metal particles and the untreated Nd-Fe-Co-based magnetic metal particles (film thickness 1.5 mm) were calculated and compared according to the line transmission theory through reflection loss (see Figure 2 ) Obtained the conclusion consistent with embodiment 1. the

实施例3:  Example 3:

与实施例1中的制备Nd-Fe-Co基磁性金属颗粒材料的方法相同,但将超声频率设置为3.5GHz,超声时长40min。将制备所得的Nd-Fe-Co基磁性金属颗粒与未作任何处理的Nd-Fe-Co基磁性金属颗粒(膜厚度1.5mm)按线传输理论经反射损耗计算并通过对比后(见图3)得到了与实施例1相一致的结论。  The method for preparing the Nd-Fe-Co-based magnetic metal particle material is the same as that in Example 1, but the ultrasonic frequency is set to 3.5 GHz, and the ultrasonic time is 40 min. The prepared Nd-Fe-Co-based magnetic metal particles and the untreated Nd-Fe-Co-based magnetic metal particles (film thickness 1.5 mm) were calculated and compared according to the line transmission theory through reflection loss (see Figure 3 ) Obtained the conclusion consistent with embodiment 1. the

Claims (1)

1.一种具有良好吸波特性的快淬Fe-基金属颗粒的制备方法,其特征是采用如下步骤: 1. A method for preparing a fast-quenching Fe-based metal particle with good wave-absorbing properties, characterized in that it adopts the following steps: Fe-基金属合金的制备:将高纯铁棒(99.9wt%)比例为65-70%、钕块(99.9wt %)比例为2-4%、分析纯钴片(99.8 wt %)比例为16-20%、分析纯硼(99.8wt%)比例为9-13%,按各元素在合金中所占的原子百分比称取相应质量的金属,配成磁性金属合金,放入高频感应熔炼炉内熔炼得到合金铸锭; The preparation of Fe-based metal alloy: the ratio of high-purity iron rod (99.9wt%) is 65-70%, the ratio of neodymium block (99.9wt%) is 2-4%, the ratio of analytical pure cobalt sheet (99.8wt%) is 16- 20%, the proportion of analytically pure boron (99.8wt%) is 9-13%, the corresponding mass of metal is weighed according to the atomic percentage of each element in the alloy, and it is made into a magnetic metal alloy, which is placed in a high-frequency induction melting furnace Smelting to obtain alloy ingots; 将(1)中所得的磁性金属合金采用真空快淬炉熔炼甩带,将合金铸锭放入坩埚,抽真空后充氩至0.05MP,在钼轮外沿线速度为20-40m/s的状态下,由钨铈电极高压电弧后将合金铸锭熔化,由高速旋转的钼轮将熔化了的溶液甩成薄带; The magnetic metal alloy obtained in (1) is smelted and thrown in a vacuum quenching furnace, and the alloy ingot is put into a crucible. After vacuuming, it is filled with argon to 0.05MP, and the speed along the outer edge of the molybdenum wheel is 20-40m/s. Next, the alloy ingot is melted by the high-voltage arc of the tungsten-cerium electrode, and the molten solution is thrown into a thin strip by the high-speed rotating molybdenum wheel; 将(2)中所得的薄带先用粉碎机粗碎,再用行星球磨机加入无水乙醇细磨,球料比10:1,转速500r/min,每20min反转一次,球磨时间为2h,将球磨2h后的磨料阴干; The thin ribbon obtained in (2) is first coarsely crushed with a pulverizer, and then finely ground with anhydrous ethanol with a planetary ball mill. The ball-to-material ratio is 10:1, the speed is 500r/min, reversed every 20min, and the ball milling time is 2h. Dry the abrasive after ball milling for 2 hours; 将(3)中所得的磨料放入烧杯中并加入适量无水乙醇,用玻璃棒充分搅拌均匀后,放入超声波设备水槽的正中央,其中水槽中的水高于烧杯中粉末高度;开启超声波设备,并设置超声频率2.5-3.5GHz,对样品进行超声处理20-40min; Put the abrasive obtained in (3) into a beaker and add an appropriate amount of absolute ethanol. After fully stirring with a glass rod, put it into the center of the water tank of the ultrasonic equipment, where the water in the water tank is higher than the powder height in the beaker; turn on the ultrasonic wave equipment, and set the ultrasonic frequency to 2.5-3.5GHz, and ultrasonically treat the sample for 20-40min; 将(4)中所得的磨料放入烘箱烘干后过筛,得到目数为200-300目的均匀Fe-基金属粉末颗粒。 The abrasive obtained in (4) is dried in an oven and then sieved to obtain uniform Fe-based metal powder particles with a mesh size of 200-300 mesh.
CN2011104408270A 2011-12-26 2011-12-26 Preparation method for quickly quenched Fe-based metal grain with excellent wave absorbing property Pending CN102528052A (en)

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