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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preparation
absorbing property
alloy
based metal
ratio
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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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Hohai University HHU
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Abstract

The invention provides a preparation method for a quickly quenched Fe-based metal grain with an excellent wave absorbing property. The preparation method comprises the following steps: weighting corresponding metals according to the mass percent of each metal element in an alloy; preparing the metals into a magnetic metal alloy; and after melting, melt-spinning and ball-milling the metal alloy, performing ultrasonic dispersing treatment, thereby obtaining a material of the Fe-based metal grain with the excellent wave absorbing property, wherein the material is capable of improving an interface property and is uniformly distributed. According to the preparation method, the cavitation principle and the mechanical effect of ultrasonic wave in liquid are utilized to obtain the uniformly distributed quickly quenched Fe-based metal grain material; and when the ultrasonic wave is transmitted in a piezoelectric material and a magnetostriction material, the wave absorbing property of the material of the Fe-based metal grain is increased due to the induced polarization and the induced magnetization caused by the mechanical effect of the ultrasonic wave. The preparation method provided by the invention is correct in principle and is scientific in measures. The material of the quickly quenched Fe-based metal grain with the excellent wave absorbing property prepared according to the preparation method is high in practical value and wide in application prospect.

Description

A kind of preparation method with fast quenching Fe-Base Metal particle of good microwave absorbing property
Technical field
The present invention relates to a kind of metallic particles material, particularly have the preparation method of the fast quenching Fe-Base Metal granular materials of good microwave absorbing property with microwave absorbing property.
Background technology
Along with development of modern science and technology, electromagenetic wave radiation increases the influence of environment day by day.On the airport, airplane flight can't take off overdue because of Electromagnetic Interference; In hospital, mobile phone regular meeting disturbs the operate as normal of various electronic instrument for diagnosing and curing diseases devices; In stealthy and electromagnetic compatibility (EMC) technology that becomes more and more important, it is very outstanding that the effect of electromagnetic wave absorbent material and status also seem, become the magic weapon and " wuwa " of electronic countermeasure in the modern military.Therefore, administer electromagnetic pollution, seek a kind of material, become a big problem of material science with good microwave absorbing property.
Absorbing material research not only militarily has great significance, and the exploitation of civil electronic industry such as anti-interference device is also played impetus.The novel design method that searching has good microwave absorbing property material is the purpose that people seek always, but absorbing material exists electromagnetic reflection problems.Though up to the present people after deliberation many electromagnetic wave absorbent materials, but still can't accomplish that areflexia absorbs, the microwave absorbing property of raising material that can only be high as far as possible is therefore apart from the still old no small distance of practical application.
Summary of the invention
The object of the present invention is to provide a kind of preparation to have the method for the fast quenching Fe-Base Metal granular materials of good microwave absorbing property, this preparation method with fast quenching Fe-Base Metal granular materials of good microwave absorbing property is characterized in that using following steps:
(1) preparation of Fe-Base Metal alloy: be that 65-70%, neodymium piece (99.9wt%) ratio are 2-4%, to analyze pure cobalt sheet (99.8wt%) ratio be 16-20%, analyze pure boron (99.8wt%) ratio with high-purity iron staff (99.9wt%) ratio be 9-13%; Take by weighing the metal of respective quality by each element shared atomic percent in alloy; Be made into the magnetic metal alloy, put into the melting of high-frequency induction smelting furnace and obtain alloy cast ingot;
(2) preparation of Fe-Base Metal strip: the magnetic metal alloy of gained in (1) is adopted the vacuum quick quenching furnace melt-spun; Alloy cast ingot is put into crucible; Vacuumize the back argon filling to 0.05MP; Linear velocity is under the state of 20-40m/s in molybdenum wheel outer, by behind the tungsten-cerium electrode high-voltage arc with the alloy cast ingot fusing, the solution that will have been melted by the molybdenum wheel of rotation at a high speed gets rid of into strip;
(3) preparation of Fe-Base Metal particle: the strip of gained in (2) is used earlier the pulverizer coarse crushing, add absolute ethyl alcohol fine grinding, ratio of grinding media to material 10: 1 with planetary ball mill again; Rotating speed 500r/min; Every 20min reverses once, and the ball milling time is 2h, and the abrasive material behind the ball milling 2h is dried in the shade;
(4) abrasive material of gained in (3) is put into beaker and added an amount of absolute ethyl alcohol, after stirring with glass bar, put into the centre of ultrasonic equipment tank, wherein the water in the tank is higher than powder height in the beaker; Open ultrasonic equipment, and supersonic frequency 2.5-3.5GHz is set, abrasive material is carried out sonicated 20-40min;
(5) sieve after the abrasive material of gained in (4) is put into oven for drying, obtaining the order number is the even Fe-based metal powder of 200-300 purpose particle.
Advantage of the present invention and effect
The Fe-based metal powder granular materials of gained in (5) is made the canonical measure ring survey its electromagnetic parameter, through finding behind the line transmission theory calculating reflection loss:
Magnetic loss μ " all has reduction by a small margin with magnetic conductivity μ ', but reduces also not obvious; Dielectric loss ε " and DIELECTRIC CONSTANTS ' obtained obvious reduction, formed better impedance matching condition, reflection loss has obtained significantly promoting, and promptly the microwave absorbing property of metallic particles material is significantly improved.
Compared with prior art; The present invention goes out to send to obtain the finely dispersed material of fast quenching Fe-Base Metal particle from utilizing the cavitation principle and the mechanical effect of ultrasonic wave liquid; When ultrasonic wave is propagated in piezoelectric and magnetostriction materials simultaneously; The polarization induced electricity and the magnetization of inducting that cause owing to hyperacoustic mechanism, thus the microwave absorbing property of Fe-Base Metal granular materials improved.The principle of the invention is correct, the means science, and a kind of piece with good microwave absorbing property that obtains with the present invention Fe-Base Metal granular materials of quenching has very high practical value, application prospects.
Description of drawings
Figure 1A is for recording the magnetic loss μ " performance plot of sample in the embodiment of the invention 1
Figure 1B is for recording the magnetic conductivity μ ' performance plot of sample in the embodiment of the invention 1
Fig. 1 C is the dielectric loss ε " performance plot that records sample in the embodiment of the invention 1
Fig. 1 D is the DIELECTRIC CONSTANTS ' performance plot that records sample in the embodiment of the invention 1
Fig. 1 E is the reflection loss performance plot that records sample in the embodiment of the invention 1
Fig. 2 is for recording the reflection loss performance plot of sample in the embodiment of the invention 2
Fig. 3 is for recording the reflection loss performance plot of sample in the embodiment of the invention 3
The specific embodiment
For a better understanding of the present invention; Following examples are further illustrated content of the present invention; Following examples are intended to explain the present invention rather than to further qualification of the present invention; Those skilled in the art makes some nonessential improvement and adjustment according to the content of the invention described above, all belongs to protection domain of the present invention.
Embodiment 1:
(1) be that 65-70%, neodymium piece (99.9wt%) ratio are 2-4%, to analyze pure cobalt sheet (99.8wt%) ratio be 16-20%, analyze pure boron (99.8wt%) ratio with high-purity iron staff (99.9wt%) ratio be 9-13%; Take by weighing the metal of respective quality by each element shared atomic percent in alloy; Be made into the magnetic metal alloy; Put into the melting of high-frequency induction smelting furnace and obtain alloy cast ingot, for guaranteeing the uniformity of composition, twice of melt back.
Adopt the vacuum quick quenching furnace melt-spun.Alloy cast ingot is put into crucible, under the state that vacuumizes the back argon filling, by behind the tungsten-cerium electrode high-voltage arc with alloy cast ingot fusing, the solution that will have been melted by the molybdenum wheel of rotation at a high speed gets rid of into strip.Then the gained ribbon is used earlier the pulverizer coarse crushing, again with drying in the shade behind the planetary ball mill adding absolute ethyl alcohol fine grinding 2h.Wherein ratio of grinding media to material is 10: 1, rotating speed 500r/min, and every 20min counter-rotating is once.
Put into the tank of ultrasonic equipment after abrasive material after will drying in the shade is poured beaker into and added an amount of absolute ethyl alcohol, open ultrasonic wave, it is 2.5GHz that supersonic frequency is set, ultrasonic duration 20min.
At last the abrasive material after ultrasonic is put into baking oven, fully sieve after the drying, obtaining the order number is the even Nd-Fe-Co-based metal powder of 200-300 purpose particle.
Basic magnetic metal particle of the Nd-Fe-Co of above preparation gained and the Nd-Fe-Co base magnetic metal particle (film thickness 1.5mm) of not doing any processing are pressed the line transmission theory to be calculated and through as shown in Figure 1 after contrasting, finds through reflection loss:
(1) after ultrasonic dispersing was handled, " reduction is by a small margin arranged, and the range of decrease was lower than 1-2% to magnetic loss μ.
(2) after ultrasonic dispersing was handled, magnetic conductivity μ ' had reduction by a small margin, and the range of decrease is lower than 1-2%.
(3) " the reduction amplitude is bigger, and when 2GHz, dielectric loss 55 is reduced to 15 by what do not deal with sample, and the range of decrease surpasses 50% for after ultrasonic dispersing is handled, dielectric loss ε.
(4) after ultrasonic dispersing is handled, DIELECTRIC CONSTANTS ' obtained obvious reduction when 2GHz, 115 is not reduced to 65 by what deal with sample, and the range of decrease surpasses 40%.
(5) after ultrasonic dispersing is handled; Reflection loss dB has obtained significantly promoting; Maximum reflection loss value before not ultrasonic by 2.2GHz-6.5dB; And the maximum reflection loss after ultrasonic reaches-11.4dB at the 3.1GHz place, has promoted with respect to the sample maximum reflection loss that does not deal with to surpass 90%.
In sum, the Nd-Fe-Co base magnetic metal particle material after handling through ultrasonic dispersing has obtained having better microwave absorbing property than the basic magnetic metal particle material of the Nd-Fe-Co that handles without ultrasonic dispersing.
Embodiment 2:
Identical with the method for preparing Nd-Fe-Co base magnetic metal particle material among the embodiment 1, but supersonic frequency is set to 3.0GHz, ultrasonic duration 30min.The Nd-Fe-Co base magnetic metal particle of preparation gained has been obtained with embodiment 1 corresponding to conclusion by the line transmission theory through reflection loss calculating and through (see figure 2) after contrasting with the Nd-Fe-Co base magnetic metal particle (film thickness 1.5mm) of not doing any processing.
Embodiment 3:
Identical with the method for preparing Nd-Fe-Co base magnetic metal particle material among the embodiment 1, but supersonic frequency is set to 3.5GHz, ultrasonic duration 40min.The Nd-Fe-Co base magnetic metal particle of preparation gained has been obtained with embodiment 1 corresponding to conclusion by the line transmission theory through reflection loss calculating and through (see figure 3) after contrasting with the Nd-Fe-Co base magnetic metal particle (film thickness 1.5mm) of not doing any processing.

Claims (1)

1. preparation method with fast quenching Fe-Base Metal particle of good microwave absorbing property is characterized in that adopting following steps:
The preparation of Fe-Base Metal alloy: be that 65-70%, neodymium piece (99.9wt %) ratio are 2-4%, to analyze pure cobalt sheet (99.8 wt %) ratio be 16-20%, analyze pure boron (99.8wt%) ratio with high-purity iron staff (99.9wt%) ratio be 9-13%; Take by weighing the metal of respective quality by each element shared atomic percent in alloy; Be made into the magnetic metal alloy, put into the melting of high-frequency induction smelting furnace and obtain alloy cast ingot;
The magnetic metal alloy of gained in (1) is adopted the vacuum quick quenching furnace melt-spun; Alloy cast ingot is put into crucible; Vacuumize the back argon filling to 0.05MP; Linear velocity is under the state of 20-40m/s in molybdenum wheel outer, by behind the tungsten-cerium electrode high-voltage arc with the alloy cast ingot fusing, the solution that will have been melted by the molybdenum wheel of rotation at a high speed gets rid of into strip;
The strip of gained in (2) is used earlier the pulverizer coarse crushing, add the absolute ethyl alcohol fine grinding with planetary ball mill again, ratio of grinding media to material 10:1, rotating speed 500r/min, every 20min reverses once, and the ball milling time is 2h, and the abrasive material behind the ball milling 2h is dried in the shade;
The abrasive material of gained in (3) is put into beaker and added an amount of absolute ethyl alcohol, after stirring with glass bar, put into the centre of ultrasonic equipment tank, wherein the water in the tank is higher than powder height in the beaker; Open ultrasonic equipment, and supersonic frequency 2.5-3.5GHz is set, sample is carried out sonicated 20-40min;
Sieve after the abrasive material of gained in (4) put into oven for drying, obtaining the order number is the even Fe-based metal powder of 200-300 purpose particle.
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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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103056354A (en) * 2013-01-09 2013-04-24 南京邮电大学 Method for preparing S-waveband composite electromagnetic wave absorption material

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CN1696211A (en) * 2004-05-11 2005-11-16 南京工业大学 Iron powder absorbent and preparation method and application thereof
CN102000816A (en) * 2010-10-27 2011-04-06 华南理工大学 Exchange coupling dual-phase nano composite permanent magnet particles and preparation method thereof
WO2011064577A1 (en) * 2009-11-27 2011-06-03 The University Of Bristol Contrast agents for medical microwave imaging

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1285896A2 (en) * 2001-08-22 2003-02-26 Kitagawa Industries Co., Ltd. Method for producing soft magnetic hexagonal ferrite sintered material and soft magnetic hexagonal ferrite sintered material
CN1696211A (en) * 2004-05-11 2005-11-16 南京工业大学 Iron powder absorbent and preparation method and application thereof
WO2011064577A1 (en) * 2009-11-27 2011-06-03 The University Of Bristol Contrast agents for medical microwave imaging
CN102000816A (en) * 2010-10-27 2011-04-06 华南理工大学 Exchange coupling dual-phase nano composite permanent magnet particles and preparation method thereof

Non-Patent Citations (3)

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Title
《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 20090315 王一凡 "聚苯胺及其复合吸波材料的制备" 第35-39页 1 , 第3期 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103056354A (en) * 2013-01-09 2013-04-24 南京邮电大学 Method for preparing S-waveband composite electromagnetic wave absorption material

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