CN102214509A - (FeCo)N microwave absorbing material and preparation method thereof - Google Patents
(FeCo)N microwave absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a novel (FeCo)N microwave absorbing material and a preparation method thereof, and relates to a novel material applied to electromagnetic wave absorption and a preparation method thereof. The (FeCo)N microwave absorbing material with 0.08 to 2.10 mass percent of N is prepared by mechanically alloying carbonyl iron powder and cobalt powder in a mass percent ratio of (50-95):(5-50), and nitriding the mechanically alloyed powder. The material has high saturation magnetization and wave absorbing property and low remanent magnetization and coercive force. The invention is characterized in that: the wave absorbing material with high saturation magnetization and wave absorbing property and low coercive force is obtained by a method for nitriding the mechanically alloyed alloy powder.
Description
Technical field
A kind of novel (FeCo) N microwave absorbing material and preparation method thereof relates to a kind of electromagnetic new material and preparation method thereof that is applied to absorb, and has higher saturation magnetization, low remanent magnetization and coercive force, the absorbing property excellence.
Background technology
Along with the continuous development of microwave communication and other microwave applications technology, the demand of traditional microwave absorbing material incompatibility modern times and following microwave technology development, the microwave absorbing material of research excellent performance is very important.
For magnetic loss type microwave absorption, high saturation and magnetic intensity and suitable coercive force are the necessary conditions that obtains high absorbing property.Adopt the synthetic FeCo alloy of method of mechanical ball milling to have high saturation and magnetic intensity, coercive force is also than the obvious raising of starting powder simultaneously.Therefore, for the synthetic FeCo alloy of the method that adopts mechanical ball milling, also need to reduce the coercive force of this absorbent.
Summary of the invention
At the shortcoming that above-mentioned absorbent exists, the objective of the invention is to propose a kind of method that adopts mechanical alloying and ammonia nitrogenize and prepared saturation magnetization height, coercive force is low and absorbing property is excellent (FeCo) N microwave absorbing material and preparation method thereof.
For achieving the above object, the present invention is achieved by the following technical solutions.
A kind of novel (FeCo) N microwave absorbing material and preparation method thereof, it is characterized in that the alloy powder after Fe powder, the mechanical alloying of Co powder is carried out the method for nitrogen treatment, obtain having high saturation and magnetic intensity, the absorbent of low-coercivity and absorbing property excellence.(FeCo) of the present invention N microwave absorbing material, be to be that 50%～95%:5%～50% carries out mechanical alloying by mass percentage with carbonyl iron dust and cobalt powder, powder after the mechanical alloying is carried out nitrogen treatment, and the N amount of containing that obtains is (FeCo) N microwave absorbing material of 0.08 quality %～2.10 quality %.
A kind of novel (FeCo) of the present invention N microwave absorbing material and preparation method thereof, it is characterized in that described mechanical alloying FeCo alloy powder, in the ball grinder of its process for the high energy ball mill of at first carbonyl iron dust of certain weight ratio and cobalt powder being packed into, after the mechanical alloying, adopt nitriding process to carry out nitrogenize and obtain the high performance microwave absorbent, and make high performance absorbing material after the mixed with resin.
Ma process is to carry out on Simoloyer (the horizontal rotor grinder of high energy) the CM01-2/ type ball mill of being made by German ZOZ GmbH Wenden company:
Ball grinder is stainless cylinder of steel, and volume is 2 liters, feeds Ar gas in the mechanical milling process with anti-oxidation, and abrading-ball is the quenching stainless steel, and average ball diameter is 2.9mm; Ball material weight ratio is 14～16: 0.5～1.5, and preferred spheres material weight ratio is 15: 1; Drum's speed of rotation is 550r/min～650r/min, and the preferred spheres mill speed is 600r/min; 18～22 hours ball milling time, the preferred spheres time consuming is 20 hours.
Adopt the synthetic FeCo alloy of method of mechanical ball milling to have high saturation and magnetic intensity, coercive force is also than the obvious raising of starting powder simultaneously.And the N element to mix Fe be that the coercive force of alloy has the reduction effect, adopt the method for nitrogenize to prepare (FeCo) N alloy microwave absorbing agent of high saturation and magnetic intensity and low-coercivity among the present invention.
The nitrogenize of FeCo alloy is to realize by vacuum/atmosphere tube type resistance furnace, adopts the technology that feeds ammonia and hydrogen nitrogenize, to the alloy powder nitrogen treatment after the mechanical alloying, obtains the absorbent of high saturation and magnetic intensity, low-coercivity and absorbing property excellence.
Description of drawings
Fig. 1 is the magnetic hysteresis loop after mechanical alloying alloy powder (FeCo) and the 450 ℃ of nitrogenize.
Fig. 2-1 is the magnetic hysteresis loop after mechanical alloying alloy powder (FeCo) and the 480 ℃ of nitrogenize.
Fig. 2-2 is the XRD analysis figure of (FeCo) N microwave absorbing material of embodiment 2 preparations.
Figure 3 shows that the magnetic hysteresis loop after mechanical alloying alloy powder (FeCo) and the 480 ℃ of nitrogenize.
Embodiment
A kind of novel (FeCo) N microwave absorbing material and preparation method thereof is characterized in that the FeCo alloy powder after the mechanical alloying is carried out the method for nitrogen treatment, obtains having high saturation and magnetic intensity, the absorbent of low-coercivity and excellent absorbing property.Preparation technology's system:
1, takes by weighing in the ball grinder of the carbonyl iron dust of certain mass ratio and cobalt powder (Co content mass percent is 5%～50%) high energy ball mill of packing into; a certain amount of stainless steel ball of packing into; ball material weight ratio is 14～16: 0.5～1.5, and preferred spheres material weight ratio is 15: 1, feeds argon shield gas.Set the ball mill program, drum's speed of rotation is 550r/min～650r/min, and the preferred spheres mill speed is 600r/min; 18～22 hours ball milling time, preferred spheres time consuming 20 hours.Mechanical milling process finishes the back and pour alcohol in ball grinder, takes out alloyed powder, dries in 58～62 ℃ of (preferred 60 ℃) baking ovens;
2, alloyed powder is put into tube type resistance furnace, carry out nitriding process, its flow process is as follows:
A, with the high temperature process furnances of packing into of the alloyed powder behind the ball milling;
B, closing device fire door with its sealing, are evacuated to below the 5Pa;
C, feeding hydrogen are opened vent valve after treating to be full of hydrogen in the stove, adjust hydrogen flowing quantity to 120～300ml/min, are heated to 375 ℃～385 ℃ rapidly, preferably are heated to 380 ℃ rapidly, are incubated 1.8～2.5 hours, preferably are incubated 2 hours;
D, be warming up to 420～510 ℃, feed ammonia, adjust hydrogen and ammonia ratio (the H2 volume is 0%～50%), be incubated 3.5～4.5 hours, preferably be incubated 4 hours;
E, when treating that fire box temperature is reduced to room temperature, stop to feed ammonia and hydrogen, nitriding process finishes;
F, close vent valve, be evacuated to below the 5Pa, feed argon gas, take out sample when treating stove internal gas pressure and extraneous balance, sample powder is carried out XRD analysis, N content measuring, VSM test.
Case study on implementation 1
Take by weighing a certain amount of carbonyl iron dust and cobalt powder, mass ratio is 3: 1, in the ball grinder of the high energy ball mill of packing into; ball material weight ratio is 15: 1, charges into argon shield gas, and drum's speed of rotation is set at 600r/min; set the ball milling program; ball milling took out after 20 hours, in the tube type resistance furnace of packing into, vacuumized the back and fed hydrogen; be heated to 380 ℃ of insulations 2 hours; be rapidly heated to 450 ℃, feed ammonia, be incubated 4 hours.
The main nitriding process parameter of FeCo alloy powder is:
Tubular electric resistance stove evacuation: 5Pa
The flow that feeds hydrogen when being heated to 380 ℃ is 300ml/min, and the flow that feeds hydrogen during 380 ℃ of insulations is 200ml/min, is incubated 2 hours.
The flow that is warming up to hydrogen after 450 ℃ is adjusted into 120ml/min, and the flow that feeds ammonia is 320ml/min, is incubated 4 hours.
Nitriding process finishes, and takes out sample, and alloy powder carries out VSM to be measured, and test result as shown in Figure 1.
Figure 1 shows that the magnetic hysteresis loop after mechanical alloying alloy powder (FeCo) and the 450 ℃ of nitrogenize, as can be seen from the figure the FeCo alloyed powder saturation magnetization through nitrogenize under 450 ℃ of conditions can reach 235.7emu/g, improved 14.64% than the FeCo alloyed powder saturation magnetization 205.6emu/g that does not adopt nitrogen treatment, and be 20Oe through the coercive force of the FeCo alloyed powder of nitrogenize under 450 ℃ of conditions, reduced by 54.54% than the FeCo alloyed powder coercive force 44Oe that does not adopt nitrogen treatment, and remanent magnetization decreases also.Illustrate that the process that the present invention proposes has good effect for improving saturation magnetization and reducing coercive force.
Adopting noble gas pulsed infrared thermal conductivity method to survey the N content results is 1.24%.
Case study on implementation 2
Take by weighing a certain amount of carbonyl iron dust and cobalt powder, mass ratio is 3: 1, puts into the ball grinder of high energy ball mill; ball material weight ratio is 15: 1, charges into argon shield gas, and drum's speed of rotation is set at 600r/min; set the ball milling program; ball milling took out after 20 hours, put into tube type resistance furnace, vacuumized the back and fed hydrogen; be heated to 380 ℃ of insulations 2 hours; be rapidly heated to 480 ℃, feed ammonia, be incubated 4 hours.
The main nitriding process parameter of FeCo alloy powder is:
Tubular electric resistance stove evacuation: 5Pa
The flow that feeds hydrogen when being heated to 380 ℃ is 300ml/min, and the flow that feeds hydrogen during 380 ℃ of insulations is 200ml/min, is incubated 2 hours.
The flow that is warming up to hydrogen after 480 ℃ is adjusted into 120ml/min, and the flow that feeds ammonia is 320ml/min, is incubated 4 hours.Nitriding process finishes, and takes out sample, and alloy powder carries out VSM to be measured, and test result is shown in Fig. 2-1.
Fig. 2-1 is depicted as the magnetic hysteresis loop after mechanical alloying alloy powder (FeCo) and the 480 ℃ of nitrogenize, as can be seen from the figure the FeCo alloyed powder saturation magnetization through nitrogenize under 480 ℃ of conditions can reach 243.8emu/g, improved 18.58% than the FeCo alloyed powder saturation magnetization 205.6emu/g that does not adopt nitrogen treatment, and be 22Oe through the coercive force of the FeCo alloyed powder of nitrogenize under 480 ℃ of conditions, reduced by 50% than the FeCo alloyed powder coercive force 44Oe that does not adopt nitrogen treatment, and remanent magnetization decreases also.Illustrate that the process that the present invention proposes has good effect for improving saturation magnetization and reducing coercive force.
Adopting noble gas pulsed infrared thermal conductivity method to survey the N content results is 1.04%.
XRD analysis is seen Fig. 2-2.
Case study on implementation 3
Take by weighing a certain amount of carbonyl iron dust and cobalt powder, mass ratio is 3: 1, puts into the ball grinder of high energy ball mill; ball material weight ratio is 15: 1, charges into argon shield gas, and drum's speed of rotation is set at 600r/min; set the ball milling program; ball milling took out after 20 hours, put into tube type resistance furnace, vacuumized the back and fed hydrogen; be heated to 380 ℃ of insulations 2 hours; be rapidly heated to 420 ℃, feed ammonia, be incubated 4 hours.
The main nitriding process parameter of FeCo alloy powder is:
Tubular electric resistance stove evacuation: 5Pa
The flow that feeds hydrogen when being heated to 380 ℃ is 300ml/min, and the flow that feeds hydrogen during 380 ℃ of insulations is 200ml/min, is incubated 2 hours.
The flow that is warming up to hydrogen after 420 ℃ is adjusted into 120ml/min, and the flow that feeds ammonia is 320ml/min, is incubated 4 hours.Nitriding process finishes, take out sample, alloy powder carries out VSM and measures, saturation magnetization is 236.1emu/g, improved 14.83% than the FeCo alloyed powder saturation magnetization 205.6emu/g that does not adopt nitrogen treatment, and coercive force is 21Oe, has reduced by 52.27% than the FeCo alloyed powder coercive force 44Oe that does not adopt nitrogen treatment, remanent magnetization is 3.709emu/g, also decreases than the FeCo alloyed powder that does not adopt nitrogen treatment.Illustrate that the process that the present invention proposes has good effect for improving saturation magnetization and reducing coercive force.
Adopting noble gas pulsed infrared thermal conductivity method to survey the N content results is 0.89%.
Case study on implementation 4
Take by weighing a certain amount of carbonyl iron dust and cobalt powder, mass ratio is 85: 15, puts into the ball grinder of high energy ball mill; ball material weight ratio is 15: 1, charges into argon shield gas, and drum's speed of rotation is set at 600r/min; set the ball milling program; ball milling took out after 20 hours, put into tube type resistance furnace, vacuumized the back and fed hydrogen; be heated to 380 ℃ of insulations 2 hours; be rapidly heated to 480 ℃, feed ammonia, be incubated 4 hours.
The main nitriding process parameter of FeCo alloy powder is:
Tubular electric resistance stove evacuation: 5Pa
The flow that feeds hydrogen when being heated to 380 ℃ is 300ml/min, and the flow that feeds hydrogen during 380 ℃ of insulations is 200ml/min, is incubated 2 hours.
The flow that is warming up to hydrogen after 480 ℃ is adjusted into 120ml/min, and the flow that feeds ammonia is 320ml/min, is incubated 4 hours.Nitriding process finishes, and takes out sample, and alloy powder carries out VSM to be measured, and test result as shown in Figure 3.
Figure 3 shows that the magnetic hysteresis loop after mechanical alloying alloy powder (FeCo) and the 480 ℃ of nitrogenize, as can be seen from the figure the FeCo alloyed powder saturation magnetization through nitrogenize under 480 ℃ of conditions can reach 231.0emu/g, improved 20.44% than the FeCo alloyed powder saturation magnetization 191.8emu/g that does not adopt nitrogen treatment, and be 26Oe through the coercive force of the FeCo alloyed powder of nitrogenize under 480 ℃ of conditions, reduced by 39.53% than the FeCo alloyed powder coercive force 43Oe that does not adopt nitrogen treatment, and remanent magnetization decreases also.Illustrate that the process that the present invention proposes has good effect for improving saturation magnetization and reducing coercive force.
Adopting noble gas pulsed infrared thermal conductivity method to survey the N content results is 1.70%.
Embodiment 5
Take by weighing a certain amount of carbonyl iron dust and cobalt powder, mass ratio is 2: 1, in the ball grinder of the high energy ball mill of packing into; ratio of grinding media to material is 15: 1; charge into argon shield gas, drum's speed of rotation is set at 600r/min, and ball milling took out after 20 hours; pack in the tube type resistance furnace; vacuumize the back and feed hydrogen, be heated to 380 ℃ of insulations 2 hours, be rapidly heated to 480 ℃; feed ammonia, be incubated 4 hours.
The main nitriding process parameter of FeCo alloy powder is:
Tubular electric resistance stove evacuation: 5Pa
The flow that feeds hydrogen when being heated to 380 ℃ is 300ml/min, and the flow that feeds hydrogen during 380 ℃ of insulations is 200ml/min, is incubated 2 hours.
The flow that is warming up to hydrogen after 480 ℃ is adjusted into 120ml/min, and the flow that feeds ammonia is 320ml/min, is incubated 4 hours.
Nitriding process finishes, take out sample, alloy powder carries out VSM and measures, saturation magnetization is 232.9emu/g, improved 18.16% than the FeCo alloyed powder saturation magnetization 197.1emu/g that does not adopt nitrogen treatment, coercive force is 24Oe, has reduced by 40% than the FeCo alloyed powder coercive force 40Oe that does not adopt nitrogen treatment, remanent magnetization is 4.345emu/g, also decreases than the FeCo alloyed powder that does not adopt nitrogen treatment.Illustrate that the process that the present invention proposes has good effect for improving saturation magnetization and reducing coercive force.
Adopting noble gas pulsed infrared thermal conductivity method to survey the N content results is 1.70%.
Case study on implementation 6
Take by weighing a certain amount of carbonyl iron dust and cobalt powder, mass ratio is 2: 1, in the ball grinder of the high energy ball mill of packing into; ratio of grinding media to material is 15: 1, charges into argon shield gas, and drum's speed of rotation is set at 600r/min; set the ball milling program; ball milling took out after 20 hours, in the tube type resistance furnace of packing into, vacuumized the back and fed hydrogen; be heated to 380 ℃ of insulations 2 hours; be rapidly heated to 480 ℃, feed ammonia, be incubated 4 hours.
The main nitriding process parameter of FeCo alloy powder is:
Tubular electric resistance stove evacuation: 5Pa
The flow that feeds hydrogen when being heated to 380 ℃ is 300ml/min, and the flow that feeds hydrogen during 380 ℃ of insulations is 300ml/min, is incubated 2 hours.
The flow that is warming up to hydrogen after 480 ℃ is adjusted into 60ml/min, and the flow that feeds ammonia is 320ml/min, is incubated 4 hours.
Nitriding process finishes, take out sample, alloy powder carries out VSM and measures, saturation magnetization can reach 224.1emu/g, improved 13.70% than the FeCo alloyed powder saturation magnetization 197.1emu/g that does not adopt nitrogen treatment, and be 22Oe through the coercive force of the FeCo alloyed powder of nitrogenize under 480 ℃ of conditions, reduced by 45% than the FeCo alloyed powder coercive force 40Oe that does not adopt nitrogen treatment, and remanent magnetization decreases also.Illustrate that the process that the present invention proposes has good effect for improving saturation magnetization and reducing coercive force.
Adopting noble gas pulsed infrared thermal conductivity method to survey the N content results is 2.08%.
Case study on implementation 7
Take by weighing a certain amount of carbonyl iron dust and cobalt powder, mass ratio is 2: 1, in the ball grinder of the high energy ball mill of packing into; ratio of grinding media to material is 15: 1, charges into argon shield gas, and drum's speed of rotation is set at 600r/min; set the ball milling program; ball milling took out after 20 hours, in the tube type resistance furnace of packing into, vacuumized the back and fed hydrogen; be heated to 380 ℃ of insulations 2 hours; be rapidly heated to 480 ℃, feed ammonia, be incubated 4 hours.
The main nitriding process parameter of FeCo alloy powder is:
Tubular electric resistance stove evacuation: 5Pa
The flow that feeds hydrogen when being heated to 380 ℃ is 300ml/min, and the flow that feeds hydrogen during 380 ℃ of insulations is 300ml/min, is incubated 2 hours.
The flow that is warming up to hydrogen after 480 ℃ is adjusted into 90ml/min, and the flow that feeds ammonia is 320ml/min, is incubated 4 hours.
Nitriding process finishes, take out sample, alloy powder carries out VSM and measures, saturation magnetization is 230.7emu/g, improved 17.05% than the FeCo alloyed powder saturation magnetization 197.1emu/g that does not adopt nitrogen treatment, coercive force is 23Oe, reduced by 42.5% than the FeCo alloyed powder coercive force 40Oe that does not adopt nitrogen treatment, and remanent magnetization decreases also.Illustrate that the process that the present invention proposes has good effect for improving saturation magnetization and reducing coercive force.
Adopting noble gas pulsed infrared thermal conductivity method to survey the N content results is 1.92%.
Can find that from above-mentioned case study on implementation FeCo alloy powder after employing that the present invention proposes is to mechanical alloying carries out the method that nitrogenize prepares New Absorbent and effectively raises the saturation magnetization of absorbent, and reduce coercive force.After the alloy powder nitrogenize after the mechanical alloying, its saturation magnetization can be more a lot of than improving before the nitrogenize after tested, and coercive force reduces.Therefore the absorbent of the present invention's preparation has high saturation and magnetic intensity, low-coercivity, is applied to absorbing material and can obtains excellent absorbing property.
Claims (3)
1. (FeCo) N microwave absorbing material, it is characterized in that, with carbonyl iron dust and cobalt powder is to carry out mechanical alloying at 50%～95%: 5%～50% by mass percentage, powder after the mechanical alloying is carried out nitrogen treatment, and the N amount of containing that obtains is (FeCo) N microwave absorbing material of 0.08 quality %～2.10 quality %.
2. the preparation method of claim 1 described (FeCo) N microwave absorption is characterized in that this preparation method comprises the steps:
(1), carbonyl iron dust and cobalt powder be to take by weighing at 50%～95%: 5%～50% by mass percentage, and in the ball grinder of the high energy ball mill of packing into, is 14～16: 0.5～1.5 stainless steel ball of packing into ball material weight ratio, feed argon shield gas and carry out ball milling;
(2), the alloyed powder behind the ball milling is carried out nitriding process, this nitriding process comprises:
A, with the high temperature process furnances of packing into of the alloyed powder behind the ball milling;
B, with high temperature process furnances sealing, be evacuated to below the 5Pa;
C, feeding hydrogen are opened vent valve after treating to be full of hydrogen in the stove, adjust hydrogen flowing quantity to 120～300ml/min, are heated to 375 ℃～385 ℃ rapidly, are incubated 1.8～2.5 hours;
Be warming up to 420～510 ℃ after d, the insulation, feed ammonia, the volume hundred of adjusting hydrogen and ammonia is incubated 3.5～4.5 hours than being 0%～50%: 50%～100%;
Stop heating after e, the insulation,, when the fire box temperature for the treatment of high temperature process furnances is reduced to room temperature, stop to feed ammonia and hydrogen with stove cooling;
F, close vent valve, be evacuated to below the 5Pa, feed argon gas, the taking-up alloyed powder promptly obtains (FeCo) N microwave absorption when treating stove internal gas pressure and extraneous balance.
3. the preparation method of (FeCo) according to claim 1 N microwave absorption is characterized in that in described step (1), drum's speed of rotation is 550r/min～650r/min, 18～22 hours ball milling time.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102416467A (en) * | 2011-11-09 | 2012-04-18 | 中国科学院金属研究所 | Metal-semiconductor electromagnetic wave absorption type nano composite material and preparation method thereof |
| CN103551568A (en) * | 2013-11-13 | 2014-02-05 | 北京科技大学 | Preparation method for scale-like nanocrystalline high temperature microwave absorbent |
| CN103752816A (en) * | 2013-12-28 | 2014-04-30 | 扬州立德粉末冶金股份有限公司 | Gasoline engine exhaust valve seat and preparing method thereof |
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| EP1548760A2 (en) * | 2003-11-27 | 2005-06-29 | Dowa Mining Co., Ltd. | Iron nitride magnetic powder and method of producing the powder |
| CN101607701A (en) * | 2009-07-24 | 2009-12-23 | 东北大学 | Nanometer, the two promotion law of high-intensity magnetic field prepare the method and the device of iron nitride material |
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| JP5009511B2 (en) * | 2005-06-06 | 2012-08-22 | 富士通株式会社 | Electrical connection structure, manufacturing method thereof, and semiconductor integrated circuit device |
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| JPH059511A (en) * | 1991-07-04 | 1993-01-19 | Mitsubishi Materials Corp | Production of fe-co soft magnetic powder |
| EP1548760A2 (en) * | 2003-11-27 | 2005-06-29 | Dowa Mining Co., Ltd. | Iron nitride magnetic powder and method of producing the powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102416467A (en) * | 2011-11-09 | 2012-04-18 | 中国科学院金属研究所 | Metal-semiconductor electromagnetic wave absorption type nano composite material and preparation method thereof |
| CN102416467B (en) * | 2011-11-09 | 2013-09-04 | 中国科学院金属研究所 | Preparation method of metal-semiconductor electromagnetic wave absorption type nano composite material |
| CN103551568A (en) * | 2013-11-13 | 2014-02-05 | 北京科技大学 | Preparation method for scale-like nanocrystalline high temperature microwave absorbent |
| CN103752816A (en) * | 2013-12-28 | 2014-04-30 | 扬州立德粉末冶金股份有限公司 | Gasoline engine exhaust valve seat and preparing method thereof |
| CN103752816B (en) * | 2013-12-28 | 2016-03-09 | 扬州立德粉末冶金股份有限公司 | A kind of gasoline engine delivery valve seat and preparation method thereof |
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