CN103803512A - Tetramanganese nitride, preparation method of tetramanganese nitride, absorbent containing tetramanganese nitride and preparation method of absorbent - Google Patents
Tetramanganese nitride, preparation method of tetramanganese nitride, absorbent containing tetramanganese nitride and preparation method of absorbent Download PDFInfo
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Abstract
The invention discloses tetramanganese nitride, a preparation method of tetramanganese nitride, an absorbent containing tetramanganese nitride and a preparation method of absorbent, wherein the absorbent is composed of micron-sized tetramanganese nitride and solid paraffin; the preparation method of the absorbent containing tetramanganese nitride comprises the steps of reacting in a tube type resistance furnace to obtain tetramanganese nitride, crushing and grinding the tetramanganese nitride in an agate mortar, and filtering through a 400-mesh screen to obtain the micron-sized tetramanganese nitride powder, and then evenly mixing the prepared micron-sized tetramanganese nitride with the paraffin at a mass ratio of (2-4):1 to obtain the absorbent. The 200-mesh electrolytic manganese powder is taken as the raw material and ammonia gas is taken as a nitrogen source, the reaction rate is increased and the reaction time is greatly reduced. The tetramanganese nitride and the absorbent can be widely popularized in the fields such as the cross technology of material science and electromagnetic theory.
Description
Technical field
The invention belongs to the interleaving techniques field of Materials science and Electromagnetic theory, relate to the technology of preparing of New Absorbent magnetic powder, absorption agent that relates to specifically a kind of nitrogenize four manganese and preparation method thereof and contain this kind of nitrogenize four manganese and preparation method thereof.
Background technology
Electromagnetic wave absorbent material is extensive application aspect stealthy technique, electromagnetic compatibility and hertzian wave physical protection, along with going deep into absorbing material research, broadband, minimal thickness, light weight, strong absorption, the contour performance of environmental compatibility have become current researchdevelopment direction, wherein, absorption agent is mainly that the electromagnetic energy that incident is come changes other forms of energy into, play main suction ripple effect, caused various countries investigators' great attention.Traditional magnetic absorbent is take ferrite, iron powder etc. as representative, but they have again different shortcomings conventionally separately, such as the ferritic low frequency scope of application, iron powder poor high temperature stability, easy to wear and perishable performance etc., range of application is subject to certain limitation.Thereby, must research and develop there is high frequency adaptability, light weight, environment resistant magnetic absorbent, in the severe environment for use in high temperature, wearing and tearing.
Nitrogenize four manganese are as a kind of nitride with essential industry purposes, and it strengthens toughness reinforcing performance, abrasion resistance properties, chemical property, make it show superior practical value and commercial value in fields such as metallurgy, electrochemistry.Recently find for the research of good magnetic absorbent, high saturation magnetization and low coercive force are the assurances that obtains high performance magnetic absorption agent.Nitrogenize four manganese are as unique a kind of nitrogenized manganese material with ferrimagnetism, and it has higher saturation magnetization and lower coercive force, and higher temperature stability and wear resisting property in addition makes it possess the potentiality as excellent magnetic wave absorbing agent.
The purposes of industrial nitrogenized manganese is mainly the main additive of iron and steel nitrogen pick-up, thereby improve the utilization ratio of manganese element and nitrogen element, improve intensity, hardness, toughness, creep resistance and the corrosion resistance of steel, thus pursue its high itrogen content of getter with nitrogen doped, nitrogenized manganese composition mainly with high nitrogen phase η and
θbe main.But the report of preparing this respect at high Magnetic Phase nitrogenize four manganese is dabbled less, visible is prepared scheme article the Chunlei Li(Journal of Alloys and Compounds of Nanjing University, 2008(457): 57 – 60) adopt solid and gas reaction method to react manganese sheet, pure nitrogenize four manganese phases are prepared, flow is 100ml/min, adopts NH
3/ N
2(volume ratio 5:95), reaction at 900 ℃.What but its raw material adopted is manganese sheet (quality is 2g), and adopt the method for nitriding, therefore speed of reaction is slow, reaction times reaches 4h, if want to improve output, need to improve the quality of manganese sheet, this must cause the reaction times of more growing, on the other hand, in the mensuration process of electromagnetic parameter, the content of wave absorbing agent nitrogenize four manganese adds too much, the paraffin nitrogenize four manganese phases that cannot bond are completely caused, greatly reduce the practicality of product, and test frequency range be only 2-12GHz, test frequency range narrow.The W.J.Feng(Solid State Communications2008(148 of Shenyang Normal University) 199 – 202) adopt thin manganese powder to do presoma, by manganese sheet under the high energy ball mill of the ball milling ratio of 40:1 after ball milling 5h, at 300 ℃, homogenizing is processed 30min, then pass into and at 550 ℃ of nitrogen, react 10s and prepared nitrogenize four manganese phases, required time is short, but need to use ball mill, the equipment such as glove box, and experiment whole process is all carried out in glove box, complicated process of preparation is not carried out electromagnetic wave absorption performance study to nitrogenize four manganese of preparation simultaneously mutually.Summary of the invention
For the problems referred to above, the invention provides a kind of speed of response fast, simple a kind of nitrogenize four manganese of preparation technology and preparation method thereof and absorption agent of containing this kind of nitrogenize four manganese and preparation method thereof.
The technique means that the present invention adopts is as follows:
A preparation method for nitrogenize four manganese, is characterized in that having following steps:
(1) take purity >=99.99%, grain graininess≤200 object electrolytic manganese powder, and described electrolytic manganese powder is put in container;
(2) described container is put in tube type resistance furnace, passed into protection gas 30-60min to get rid of quartzy inner air tube with the flow of 400-600ml/min;
(3) tube type resistance furnace is heated up;
(4), in the time that furnace temperature rises to 800-1000 ℃, close protection gas; Flow with 37.5-300ml/min passes into ammonia, and to keep tubular type furnace gas pressure be 0.1-0.3MPa;
(5) after insulation 10min-4h, stop tube type resistance furnace heating; Silica tube is released simultaneously, at room temperature cooling, in the time that furnace temperature is down to 300 ℃, stop passing into ammonia gas, and pass into protection gas; In the time that furnace temperature is down to below 100 ℃, described container is taken out, collect product and obtain nitrogenize four manganese.
Further, in described step (2), (4) and (5), protection gas is one or more in argon gas, helium, neon.
Further, in described step (4), keeping gas pressure intensity in silica tube is 0.2MPa.
Further, in described step (5), soaking time is 1h-4h; Further, in described step (5), soaking time is 2h.
Further, in described step (1), (2) and (5), container is the one in porcelain boat, quartz boat or crucible.
A kind of nitrogenize four manganese, it is prepared from by the preparation method of aforesaid a kind of nitrogenize four manganese.
A preparation method for nitrogenize four manganese absorption agents, is characterized in that having following steps:
(1) by aforesaid a kind of nitrogenize four manganese crushing grindings, and 400 eye mesh screens obtain micron order nitrogenize four manganese powder ends excessively;
(2) the micron order nitrogenize four manganese powder ends that above-mentioned steps (1) obtained mix according to mass ratio 2-4:1 with solid paraffin, in the time that micron order nitrogenize four manganese powder ends are less than 2:1 with solid paraffin mass ratio, prepared absorption agent reflectivity is high, does not possess absorbing property; In the time that micron order nitrogenize four manganese powder ends are greater than 4:1 with solid paraffin mass ratio, solid paraffin and micron order nitrogenize four manganese powder ends cannot mix.
Further, in described step (2), nitrogenize four manganese mix according to mass ratio 3:1 with solid paraffin.
It is Ф 7mm that the described a kind of nitrogenize four manganese absorption agents that obtain after above-mentioned steps are pressed into external diameter, and internal diameter is Ф 3mm, in the coaxial die that thickness is 2mm, thereby obtains testing sample.
Utilize coaxial method, on vector network analyzer, described testing sample is carried out to electromagnetic performance test.
A kind of nitrogenize four manganese absorption agents, it is prepared from by the preparation method of aforesaid a kind of nitrogenize four manganese absorption agents.
The present invention has the following advantages:
1, adopt grain graininess≤200 object electrolytic manganese powder as raw material, ammonia, as nitrogenous source, has increased speed of reaction, has greatly reduced the reaction times.
2, after stopping tube type resistance furnace heating, silica tube is released from tube type resistance furnace, made to react rear sample at room temperature cooling, accelerated rate of temperature fall, reduced nitrogen pick-up and the oxidation of sample in temperature-fall period, guaranteed constant product quality.
The present invention can extensively promote in fields such as the interleaving techniquess of Materials science and Electromagnetic theory for the foregoing reasons.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of nitrogenize four manganese of synthesized in the embodiment of the present invention 1.
Fig. 2 is the SEM figure of nitrogenize four manganese of synthesized in the embodiment of the present invention 1.
Fig. 3 is the saturation magnetization curve of nitrogenize four manganese of synthesized in the embodiment of the present invention 1.
Fig. 4 is magnetic permeability-frequency collection of illustrative plates of the absorption agent of synthesized in the embodiment of the present invention 1.
Fig. 5 is absorptive character-frequency collection of illustrative plates of the absorption agent of synthesized in the embodiment of the present invention 1.
Fig. 6 is X-ray diffraction (XRD) collection of illustrative plates of nitrogenize four manganese of synthesized in the embodiment of the present invention 2.
Fig. 7 is the SEM figure of nitrogenize four manganese of synthesized in the embodiment of the present invention 2.
Fig. 8 is the saturation magnetization curve of nitrogenize four manganese of synthesized in the embodiment of the present invention 2.
Fig. 9 is magnetic permeability-frequency collection of illustrative plates of the absorption agent of synthesized in the embodiment of the present invention 2.
Figure 10 is absorptive character-frequency collection of illustrative plates of the absorption agent of synthesized in the embodiment of the present invention 2.
Figure 11 is X-ray diffraction (XRD) collection of illustrative plates of nitrogenize four manganese of synthesized in the embodiment of the present invention 3.
Figure 12 is the SEM figure of nitrogenize four manganese of synthesized in the embodiment of the present invention 3.
Figure 13 is the saturation magnetization curve of nitrogenize four manganese of synthesized in the embodiment of the present invention 3.
Figure 14 is magnetic permeability-frequency collection of illustrative plates of the absorption agent of synthesized in the embodiment of the present invention 3.
Figure 15 is absorptive character-frequency collection of illustrative plates of the absorption agent of synthesized in the embodiment of the present invention 3.
Figure 16 is X-ray diffraction (XRD) collection of illustrative plates of nitrogenize four manganese of synthesized in the embodiment of the present invention 4.
Figure 17 is the SEM figure of nitrogenize four manganese of synthesized in the embodiment of the present invention 4.
Figure 18 is the saturation magnetization curve of nitrogenize four manganese of synthesized in the embodiment of the present invention 4.
Figure 19 is magnetic permeability-frequency collection of illustrative plates of the absorption agent of synthesized in the embodiment of the present invention 4.
Figure 20 is absorptive character-frequency collection of illustrative plates of the absorption agent of synthesized in the embodiment of the present invention 4.
Embodiment
It is below the example of a kind of nitrogenize four manganese absorption agents of preparation.
Embodiment 1:
1, take with electronic balance that 4g purity is 99.99%, grain graininess is 200 object electrolytic manganese powders, and described electrolytic manganese powder is put in porcelain boat.
2, described porcelain boat is put into the central position of tube type resistance furnace, in silica tube, passed into argon shield gas 30min with the flow of 600ml/min, to get rid of the air in silica tube.
4, tube type resistance furnace is heated up, continue to pass into argon gas simultaneously.
5, in the time that furnace temperature rises to 900 ℃, close argon gas, simultaneously pass into ammonia with the flow of 100ml/min, and to keep gas pressure intensity in silica tube be 0.2Mpa.
6, after insulation 2h, stop tube type resistance furnace heating; Silica tube is released from tube type resistance furnace, at room temperature cooling; In the time being cooled to 300 ℃, stop passing into ammonia gas, and pass into argon gas with the flow of 400ml/min, in order to avoid hydrogen content is too high, set off an explosion, in the time that temperature is down to below 100 ℃, porcelain boat is taken out, collect product and obtain nitrogenize four manganese.
7, described nitrogenize four manganese are placed on to crushing grinding in agate mortar, and through 400 eye mesh screen screenings.
8, be 0.87g/cm by described micron-sized nitrogenize four manganese and density
3solid paraffin mix by the mass ratio of 3:1, obtain described a kind of nitrogenize four manganese absorption agents.
It is Ф 7mm that the described a kind of nitrogenize four manganese absorption agents that obtain after above-mentioned steps are pressed into external diameter, internal diameter is Ф 3mm, thickness is in the coaxial die of 2mm, obtain testing sample, the filling ratio of filler is 75wt%, measures complex permittivity and the complex permeability of described a kind of nitrogenize four manganese absorption agents and calculate its theoretical absorbing property under vector network analyzer.
Fig. 1 is the XRD figure of nitrogenize four manganese that obtain of embodiment 1, by mainly containing nitrogenize four manganese in known this material of diffraction peak in figure, also has in addition a small amount of excessively ζ-Mn of nitrogenize
2n
0.86with a small amount of manganese monoxide.
Fig. 2 is the SEM figure of nitrogenize four manganese that obtain of embodiment 1, and these nitrogenize four manganese particles have irregular bulk morphologies as seen from the figure, are of a size of micron order.
Fig. 3 is the static magnetization VSM figure of nitrogenize four manganese that obtain of embodiment 1, and the saturation magnetization of these nitrogenize four manganese is 17.79emu/g as seen from the figure, and coercive force is 69Oe.
Fig. 4 is the magnetic permeability figure of the absorption agent that obtains of embodiment 1, has the magnetic permeability of known this absorption agent of figure under microwave section 2-6GHz, to have higher magnetic permeability imaginary part, the highlyest can reach 0.34.
Fig. 5 is the 6mm microwave absorbing property calculation result of the absorption agent that obtains of embodiment 1, there are two absorption peaks in this absorption agent as seen from the figure, the frequency range that is greater than 10dB is respectively 3.9-4.6GHz and 12.72-14.76Ghz, wherein, under 13.49GHz, occurs maximum absorption peak-26dB.
Embodiment 2:
1, take with electronic balance that 4g purity is 99.99%, grain graininess is 200 object electrolytic manganese powders, and described electrolytic manganese powder is put in porcelain boat.
2, described porcelain boat is put into the central position of tube type resistance furnace, in silica tube, passed into argon shield gas 30min with the flow of 600ml/min, to get rid of the air in silica tube.
4, tube type resistance furnace is heated up, continue to pass into argon gas simultaneously.
5, in the time that furnace temperature rises to 900 ℃, close argon gas, simultaneously pass into ammonia with the flow of 100ml/min, and to keep gas pressure intensity in silica tube be 0.2Mpa.
6, after insulation 4h, stop tube type resistance furnace heating; Silica tube is released from tube type resistance furnace, at room temperature cooling; In the time being cooled to 300 ℃, stop passing into ammonia gas, and pass into argon gas with the flow of 400ml/min, in order to avoid hydrogen content is too high, set off an explosion, in the time that temperature is down to below 100 ℃, porcelain boat is taken out, collect product and obtain nitrogenize four manganese.
7, described nitrogenize four manganese are placed on to crushing grinding in agate mortar, and through 400 eye mesh screen screenings.
8, be 0.87g/cm by described micron-sized nitrogenize four manganese and density
3solid paraffin mix by the mass ratio of 3:1, obtain described a kind of nitrogenize four manganese absorption agents.
It is Ф 7mm that the described a kind of nitrogenize four manganese absorption agents that obtain after above-mentioned steps are pressed into external diameter, internal diameter is Ф 3mm, thickness is in the coaxial die of 2mm, obtain testing sample, the filling ratio of filler is 75wt%, measures complex permittivity and the complex permeability of described a kind of nitrogenize four manganese absorption agents and calculate its theoretical absorbing property under vector network analyzer.
Fig. 6 is the XRD figure of nitrogenize four manganese that obtain of embodiment 2, by mainly containing nitrogenize four manganese in known this material of diffraction peak in figure, also has in addition a small amount of excessively ζ-Mn of nitrogenize
2n
0.86with a small amount of manganese monoxide.
Fig. 7 is the SEM figure of nitrogenize four manganese that obtain of embodiment 2, and these nitrogenize four manganese particles have irregular bulk morphologies as seen from the figure, are of a size of micron order.
Fig. 8 is the static magnetization VSM figure of nitrogenize four manganese that obtain of embodiment 2, and the saturation magnetization of these nitrogenize four manganese is 15.83emu/g as seen from the figure, and coercive force is 54Oe.
Fig. 9 is the magnetic permeability figure of the absorption agent that obtains of embodiment 2, has the magnetic permeability of known this absorption agent of figure under microwave section 2-6GHz, to have higher magnetic permeability imaginary part, can reach 0.25 2.25GHz magnetic permeability imaginary values is the highest.
Figure 10 is the 5mm microwave absorbing property calculation result of the absorption agent that obtains of embodiment 2, there are two absorption peaks in this absorption agent as seen from the figure, the frequency range that is greater than 10dB is respectively 4.4-4.85GHz and 13.82-15.03Ghz, wherein, under 14.48GHz, occurs maximum absorption peak-22dB.
Embodiment 3:
1, take with electronic balance that 4g purity is 99.99%, grain graininess is 200 object electrolytic manganese powders, and described electrolytic manganese powder is put in porcelain boat.
2, described porcelain boat is put into the central position of tube type resistance furnace, in silica tube, passed into argon shield gas 30min with the flow of 600ml/min, to get rid of the air in silica tube.
4, tube type resistance furnace is heated up, continue to pass into argon gas simultaneously.
5, in the time that furnace temperature rises to 900 ℃, close argon gas, simultaneously pass into ammonia with the flow of 100ml/min, and to keep gas pressure intensity in silica tube be 0.2MPa.
6, after insulation 10min, stop tube type resistance furnace heating; Silica tube is released from tube type resistance furnace, at room temperature cooling; In the time being cooled to 300 ℃, stop passing into ammonia gas, and pass into argon gas with the flow of 400ml/min, in order to avoid hydrogen content is too high, set off an explosion, in the time that temperature is down to below 100 ℃, porcelain boat is taken out, collect product and obtain nitrogenize four manganese.
7, described nitrogenize four manganese are placed on to crushing grinding in agate mortar, and through 400 eye mesh screen screenings.
8, be 0.87g/cm by described micron-sized nitrogenize four manganese and density
3solid paraffin mix by the mass ratio of 3:1, obtain described a kind of nitrogenize four manganese absorption agents.
It is Ф 7mm that the described a kind of nitrogenize four manganese absorption agents that obtain after above-mentioned steps are pressed into external diameter, internal diameter is Ф 3mm, thickness is in the coaxial die of 2mm, obtain testing sample, the filling ratio of filler is 75wt%, measures complex permittivity and the complex permeability of described a kind of nitrogenize four manganese absorption agents and calculate its theoretical absorbing property under vector network analyzer.
Figure 11 is the XRD figure of nitrogenize four manganese that obtain of embodiment 3, by mainly containing nitrogenize four manganese and a small amount of manganese monoxide in known this material of diffraction peak in figure.
Figure 12 is the SEM figure of nitrogenize four manganese that obtain of embodiment 3, and these nitrogenize four manganese particles have irregular bulk morphologies as seen from the figure, are of a size of micron order.
Figure 13 is the static magnetization VSM figure of nitrogenize four manganese that obtain of embodiment 3, and the saturation magnetization of these nitrogenize four manganese is 11.7emu/g as seen from the figure, and coercive force is 85Oe.
Figure 14 is the magnetic permeability figure of the absorption agent that obtains of embodiment 3, and the magnetic permeability of this absorption agent has higher magnetic permeability imaginary part under microwave section 2-6GHz as seen from the figure, the highlyest can reach 0.2.
Figure 15 is the 6mm microwave absorbing property calculation result of the absorption agent that obtains of embodiment 3, and two absorption peaks appear in this absorption agent as seen from the figure, and the frequency range that is greater than 10dB is 12.6-13.8Ghz, wherein, under 12.27GHz, occurs maximum absorption peak-18.57dB.
Embodiment 4:
1, take with electronic balance that 4g purity is 99.99%, grain graininess is 200 object electrolytic manganese powders, and described electrolytic manganese powder is put in porcelain boat.
2, described porcelain boat is put into the central position of tube type resistance furnace, in silica tube, passed into argon shield gas 30min with the flow of 600ml/min, to get rid of the air in silica tube.
4, tube type resistance furnace is heated up, continue to pass into argon gas simultaneously.
5, in the time that furnace temperature rises to 900 ℃, close argon gas, simultaneously pass into ammonia with the flow of 100ml/min, and to keep gas pressure intensity in silica tube be 0.2Mpa.
6, after insulation 1h, stop tube type resistance furnace heating; Silica tube is released from tube type resistance furnace; In the time being cooled to 300 ℃, stop passing into ammonia gas, and pass into argon gas with the flow of 400ml/min, in order to avoid hydrogen content is too high, set off an explosion, in the time that temperature is down to below 100 ℃, porcelain boat is taken out, collect product and obtain nitrogenize four manganese.
7, described nitrogenize four manganese are placed on to crushing grinding in agate mortar, and through 400 eye mesh screen screenings.
8, be 0.87g/cm by described micron-sized nitrogenize four manganese and density
3solid paraffin mix by the mass ratio of 3:1, obtain described a kind of nitrogenize four manganese absorption agents.
It is Ф 7mm that the described a kind of nitrogenize four manganese absorption agents that obtain after above-mentioned steps are pressed into external diameter, internal diameter is Ф 3mm, thickness is in the coaxial die of 2mm, obtain testing sample, the filling ratio of filler is 75wt%, measures complex permittivity and the complex permeability of described a kind of nitrogenize four manganese absorption agents and calculate its theoretical absorbing property under vector network analyzer.
Figure 16 is the XRD figure of nitrogenize four manganese that obtain of embodiment 4, by mainly containing nitrogenize four manganese in known this material of diffraction peak in figure, also has in addition a small amount of excessively ζ-Mn of nitrogenize
2n
0.86with a small amount of manganese monoxide.
Figure 17 is the SEM figure of nitrogenize four manganese that obtain of embodiment 4, and these nitrogenize four manganese particles have irregular bulk morphologies as seen from the figure, are of a size of micron order.
Figure 18 is the static magnetization VSM figure of nitrogenize four manganese that obtain of embodiment 4, and the saturation magnetization of these nitrogenize four manganese is 15.36emu/g as seen from the figure, and coercive force is 79Oe.
Figure 19 is the magnetic permeability figure of the absorption agent that obtains of embodiment 4, has the magnetic permeability of known this absorption agent of figure under microwave section 2-6GHz, to have higher magnetic permeability imaginary part, the highlyest can reach 0.2.
Figure 20 is the 6mm microwave absorbing property calculation result of the absorption agent that obtains of embodiment 4, and two absorption peaks appear in this absorption agent as seen from the figure, and the frequency range that is greater than 10dB is 12.6-13.8Ghz, wherein, under 12.27GHz, occurs maximum absorption peak-18.57dB.
The above; it is only preferably embodiment of the present invention; but protection scope of the present invention is not limited to this; any be familiar with those skilled in the art the present invention disclose technical scope in; be equal to replacement or changed according to technical scheme of the present invention and inventive concept thereof, within all should being encompassed in protection scope of the present invention.
Claims (9)
1. a preparation method for nitrogenize four manganese, is characterized in that having following steps:
(1) take purity >=99.99%, grain graininess≤200 object electrolytic manganese powder, and described electrolytic manganese powder is put in container;
(2) described container is put in tube type resistance furnace, passed into protection gas to get rid of quartzy inner air tube;
(3) tube type resistance furnace is heated up;
(4), in the time that furnace temperature rises to 800-1000 ℃, close protection gas; Pass into ammonia, and to keep gas pressure intensity in silica tube be 0.10MPa-0.30MPa;
(5) after insulation 10min-4h, stop tube type resistance furnace heating; Silica tube is released simultaneously, at room temperature cooling, in the time that furnace temperature is down to 300 ℃, stop passing into ammonia gas, and pass into protection gas; In the time that furnace temperature is down to below 100 ℃, described container is taken out, collect product and obtain nitrogenize four manganese.
2. the preparation method of a kind of nitrogenize four manganese according to claim 1, is characterized in that: in described step (2), (4) and (5), protection gas is one or more in argon gas, helium, neon.
3. the preparation method of a kind of nitrogenize four manganese according to claim 1, is characterized in that: in described step (4), keeping gas pressure intensity in silica tube is 0.2MPa.
4. the preparation method of a kind of nitrogenize four manganese according to claim 1, is characterized in that: in described step (5), soaking time is 1h-4h.
5. the preparation method of a kind of nitrogenize four manganese according to claim 1, is characterized in that: in described step (1), (2) and (5), container is the one in porcelain boat, quartz boat or crucible.
6. nitrogenize four manganese, it is prepared from by the preparation method of arbitrary described a kind of nitrogenize four manganese of claim 1 to 5.
7. a preparation method for nitrogenize four manganese absorption agents, is characterized in that having following steps:
(1) by a kind of nitrogenize four manganese crushing grindings claimed in claim 6, and 400 eye mesh screens obtain micron order nitrogenize four manganese powder ends excessively;
(2) the micron order nitrogenize four manganese powder ends that above-mentioned steps (1) obtained mix according to mass ratio 2-4:1 with solid paraffin.
8. the preparation method of a kind of nitrogenize four manganese absorption agents according to claim 7, is characterized in that: in described step (2), nitrogenize four manganese mix according to mass ratio 3:1 with solid paraffin.
9. nitrogenize four manganese absorption agents, it is prepared from by the preparation method of a kind of nitrogenize four manganese absorption agents described in claim 7 or 8.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101082088A (en) * | 2006-11-06 | 2007-12-05 | 王国宁 | Production technique for preparing high-purity high-nitrogen nitrogenization manganese metal |
| CN101172586A (en) * | 2007-09-30 | 2008-05-07 | 冯良荣 | Method for producing manganese nitride |
| CN103112834A (en) * | 2012-10-17 | 2013-05-22 | 浙江欣万飞科技有限公司 | Method for preparing ultra-high manganese nitride |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101082088A (en) * | 2006-11-06 | 2007-12-05 | 王国宁 | Production technique for preparing high-purity high-nitrogen nitrogenization manganese metal |
| CN101172586A (en) * | 2007-09-30 | 2008-05-07 | 冯良荣 | Method for producing manganese nitride |
| CN103112834A (en) * | 2012-10-17 | 2013-05-22 | 浙江欣万飞科技有限公司 | Method for preparing ultra-high manganese nitride |
Non-Patent Citations (1)
| Title |
|---|
| 张金柱等: "金属锰氮化的动力学研究", 《铁合金》, no. 3176, 31 December 2004 (2004-12-31), pages 9 - 12 * |
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