CN104831173A - Preparation method of chromium-doped ferrous alloy wave-absorbing material - Google Patents

Preparation method of chromium-doped ferrous alloy wave-absorbing material Download PDF

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Publication number
CN104831173A
CN104831173A CN201510228720.8A CN201510228720A CN104831173A CN 104831173 A CN104831173 A CN 104831173A CN 201510228720 A CN201510228720 A CN 201510228720A CN 104831173 A CN104831173 A CN 104831173A
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absorbing material
sample
alloy
preparation
chromium
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黄鹏腾
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Abstract

The invention relates to a preparation method of a chromium-doped ferrous alloy wave-absorbing material. The preparation method comprises the following steps: mixing raw materials: Fe, Nd and Cr according to a certain atom ratio, melting the metals in an arc furnace; then sealing the alloy sample in a vacuum quartz glass tube, then placing the sealed quartz glass tube in a high-temperature environment to carry out a further homogenization treatment, quenching, taking out the alloy sample, mechanically and primarily grinding the alloy sample in a mortar, then transferring the alloy powder to a stainless steel ball-milling tank, carrying out high-energy ball milling under the protection of gasoline, after a while, pouring out the gasoline, taking out the alloy sample powder, drying the powder in the air so as to obtain the alloy micropowder wave-absorbing material.

Description

A kind of preparation method of chromium-doped ferrous alloy absorbing material
Technical field
The present invention relates to a kind of method utilizing alloy powder to prepare absorbing material, particularly a kind of preparation method of chromium-doped ferrous alloy absorbing material.
Background technology
Along with electronization, informationalized development, the hertzian wave that a large amount of electronic product produces disturbs mutually, can cause communication disruption, the serious problems such as equipment malfunction.Along with stealth technique and the stealthy development equipped in military affairs, stealth material must promote accelerated development that is stealthy and anti-stealth countermeasure techniques, and electromagnetic wave absorption material has become a large problem of Materials science.Microwave absorbing material as a kind of can the functional materials of electromagnetic wave absorption, electromagnetic wave energy can be converted into other forms of energy by it, suppresses electromagnetic radiation and interference with this.
Absorbing material has reached tens kinds more than, and wherein applying wider a few class absorbing materials has ferrite, metal fine powder, conduction high polymer and ferroelectric absorbing material etc.Except requiring having hertzian wave except high specific absorption in broad frequency band on engineer applied, require that material has lightweight, heatproof, moisture-proof, the performance such as anticorrosive, in numerous absorbing material, electromagnetic wave absorbing material has clear superiority, and will be main research object, electromagnetic wave absorbing material mainly comprises ferrite, super-fine metal powder, polycrystalline iron fiber, alloy powder etc.Ferrite has lower specific inductivity, and matching properties is better, but microwave magnetic permeability is not high enough, and the coating of preparation is thicker.And Metal absorption agent has the features such as use good, the saturation magnetization of high-temperature behavior and magnetic loss ability is large, metal fine powder absorbing material is mainly by the attenuation by absorption such as magnetic hysteresis loss, eddy-current loss hertzian wave.
Because the resource of Fe is abundanter, price is all cheaper relative to Co and Ni, and therefore the preparation of Fe base alloy absorbing material becomes the emphasis of research.FeNd alloy is widely studied with the absorbing property of excellence, although obtain certain achievement, but still it is desirable not enough to there is absorbing property, inhales ripple frequency band narrower.In order to overcome these shortcomings, the present invention is by doping Cr medium, and increase alloy uptake and accumulation effect, and regulate it to mate, make its absorption band broadening, maximum reflection loss increases, and finally prepares the microwave absorbing material that a kind of absorption band is wide, specific absorption is strong.
Summary of the invention
The invention provides a kind of preparation method of chromium-doped ferrous alloy absorbing material, concrete steps are realized by following technological line:
(1) metal Fe, Nd, Cr are prepared burden by certain atomic ratio;
(2) the raw material prepared is put into vacuum arc fumace and carry out melting, melting number of times is 2-3 time;
(3), after the cooling of melted alloy, take out, and be placed on vacuum-sealing in quartz glass tube;
(4) the silica tube that vacuum-sealing is good is put into water, check it whether to seal completely;
(5) again the Glass tubing that alloy sample is housed is put into stove, carry out homogenizing annealing process;
(6) after annealing for some time, sample is taken out and puts into rapidly mixture of ice and water and quench;
(7) treat that sample fully cools, and breaks Glass tubing, the sample in take-off pipe;
(8) sample is carried out in mortar machinery tentatively to pulverize;
(9), by the sample after pulverizing, pour in ball grinder, under the protection of gasoline, carry out ball milling with planetary ball mill;
(10) after ball milling for some time, alloy powder take out dry, a kind of alloy powder absorbing material.
Preferentially, step (1) in, metal Fe, metal Nd and Cr purity are greater than 99.5%, are Fe according to atomic ratio 17nd 2-xcr x(0.3≤X≤0.5) prepares burden.
Preferentially, step (5) in, annealing temperature controls at 700-900 DEG C, and annealing time is 10-15 days.
Preferentially, step (9) in, ratio of grinding media to material is 15:1-20:1, and planetary ball mill speed control 250-350 r/min runs.
Preferentially, step (10) in, the time of carrying out ball milling with planetary ball mill is 50-70h.
The present invention has following advantages and characteristic:
(1) the sorbing material produced of this method, raw material sources are extensive, and with low cost, preparation technology is simple;
(2) inhale ripple bandwidth, absorption intensity is high.
Embodiment
Embodiment one:
Metal Fe, Nd, Cr of purity being greater than 99.5% are Fe by atomic ratio 17nd 1.7cr 0.3batching.To prepare sample loads in vacuum arc fumace, through vacuumizing, ventilation scrubbing operations, in triplicate, then a certain amount of argon gas is filled with as shielding gas, start melting, each sample melting three times, melted sample is loaded in quartz glass tube, and carry out vacuum seal operative, Glass tubing is put into its stopping property of built for in-water survey, after inspection sealing is intact, Glass tubing is put into chamber type electric resistance furnace under 700 DEG C of envrionment conditionss, carries out anneal, after 15 days, Glass tubing is taken out still enter in mixture of ice and water and quench, after fully cooling, take out Glass tubing and smash, take out sample, sample surfaces layer is polished off, carry out machinery with mortar more tentatively to pulverize, ball milling is carried out with planetary ball mill after mechanical disintegration, under the protection of gasoline, with ball material mass ratio for 20:1, rotating speed is the condition of 250 r/min, ball milling 50 h, ball milling terminates rear alloy powder is taken out and dries, a kind of alloy powder absorbing material.
Embodiment two:
Metal Fe, Nd, Cr of purity being greater than 99.5% are Fe by atomic ratio 17nd 1.6cr 0.4batching.To prepare sample loads in vacuum arc fumace, through vacuumizing, ventilation scrubbing operations, in triplicate, then a certain amount of argon gas is filled with as shielding gas, start melting, each sample melting three times, melted sample is loaded in quartz glass tube, and carry out vacuum seal operative, Glass tubing is put into its stopping property of built for in-water survey, after inspection sealing is intact, Glass tubing is put into chamber type electric resistance furnace under 800 DEG C of envrionment conditionss, carries out anneal, after 12 days, Glass tubing is taken out still enter in mixture of ice and water and quench, after fully cooling, take out Glass tubing and smash, take out sample, sample surfaces layer is polished off, carry out machinery with mortar more tentatively to pulverize, ball milling is carried out with planetary ball mill after mechanical disintegration, under the protection of gasoline, with ball material mass ratio for 20:1, rotating speed is the condition of 250 r/min, ball milling 50 h, ball milling terminates rear alloy powder is taken out and dries, a kind of alloy powder absorbing material.
Embodiment three:
Metal Fe, Nd, Cr of purity being greater than 99.5% are Fe by atomic ratio 17nd 1.5cr 0.5batching.To prepare sample loads in vacuum arc fumace, through vacuumizing, ventilation scrubbing operations, in triplicate, then a certain amount of argon gas is filled with as shielding gas, start melting, each sample melting three times, melted sample is loaded in quartz glass tube, and carry out vacuum seal operative, Glass tubing is put into its stopping property of built for in-water survey, after inspection sealing is intact, Glass tubing is put into chamber type electric resistance furnace under 800 DEG C of envrionment conditionss, carries out anneal, after 12 days, Glass tubing is taken out still enter in mixture of ice and water and quench, after fully cooling, take out Glass tubing and smash, take out sample, sample surfaces layer is polished off, carry out machinery with mortar more tentatively to pulverize, ball milling is carried out with planetary ball mill after mechanical disintegration, under the protection of gasoline, with ball material mass ratio for 20:1, rotating speed is the condition of 250 r/min, ball milling 50 h, ball milling terminates rear alloy powder is taken out and dries, a kind of alloy powder absorbing material.

Claims (4)

1. a preparation method for chromium-doped ferrous alloy absorbing material, is characterized in that, this preparation method comprises the steps:
(1) purity is greater than metal Fe, Nd, Cr of 99.5% by Fe 17nd 2-xcr xthe atomic ratio batching of (0.3≤X≤0.5);
(2) the raw material prepared is put into vacuum arc fumace and carry out melting, melting number of times is 2-3 time;
(3), after the cooling of melted alloy, take out, and be placed on vacuum-sealing in quartz glass tube;
(4) the silica tube that vacuum-sealing is good is put into water, check it whether to seal completely;
(5) again the Glass tubing that alloy sample is housed is put into stove, carry out homogenizing annealing process;
(6) after annealing for some time, sample is taken out and puts into rapidly mixture of ice and water and quench;
(7) treat that sample fully cools, and breaks Glass tubing, the sample in take-off pipe;
(8) sample is carried out in mortar machinery tentatively to pulverize;
(9), by the sample after pulverizing, pour in ball grinder, under the protection of gasoline, carry out ball milling with planetary ball mill;
(10) after ball milling for some time, alloy powder take out dry, a kind of alloy powder absorbing material.
2. the preparation method of a kind of chromium-doped ferrous alloy absorbing material according to claim 1, is characterized in that, step (5) in, annealing temperature controls at 700-900 DEG C, and annealing time is 10-15 days.
3. the preparation method of a kind of chromium-doped ferrous alloy absorbing material according to claim 1, is characterized in that, step (9) in, ratio of grinding media to material is 15:1-20:1, and ball mill speed is 250-350 r/min.
4. the preparation method of a kind of chromium-doped ferrous alloy absorbing material according to claim 1, is characterized in that, step (10) in, the time of ball milling is 50-70h.
CN201510228720.8A 2015-05-07 2015-05-07 Preparation method of chromium-doped ferrous alloy wave-absorbing material Pending CN104831173A (en)

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Cited By (16)

* Cited by examiner, † Cited by third party
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CN106334798A (en) * 2016-09-09 2017-01-18 电子科技大学 Preparation method for Fe-based nanocrystalline alloy flake micropowder
CN106552949A (en) * 2015-09-30 2017-04-05 吴涵 A kind of Dy-Co-Ga types alloy inhales ripple micropowder material and preparation method thereof
CN106552947A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt alloy of addition boron inhales ripple micro mist
CN106552946A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt alloy of addition vanadium inhales the preparation method of ripple micro mist
CN106552948A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt-base alloyss of Doped with Titanium inhale the preparation technology of ripple micropowder
CN106552933A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt-base alloyss of doping Al inhale ripple micropowder and its preparation technology
CN106552934A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt alloy of addition chromium inhales ripple micropowder material
CN106552945A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt-base alloys of doping Si inhales ripple micro mist and preparation method thereof
CN106607581A (en) * 2015-10-25 2017-05-03 杨欣睿 Rare earth Ce-doped alloy wave absorbing micro powder and preparing technology thereof
CN106607593A (en) * 2015-10-25 2017-05-03 杨欣睿 Fe-Ni base alloy wave absorbing micro powder added with Tb and preparation process of Fe-Ni base alloy wave absorbing micro powder
CN106607590A (en) * 2015-10-25 2017-05-03 杨欣睿 Fe-Ni-based alloy absorbing material
CN106607580A (en) * 2015-10-25 2017-05-03 杨欣睿 A rare earth-added alloy wave absorbing material
CN106607592A (en) * 2015-10-25 2017-05-03 杨欣睿 Y-doped rare earth alloy wave absorbing micro powder and preparing method thereof
CN106607591A (en) * 2015-10-25 2017-05-03 杨欣睿 Fe-Ni-based alloy absorbing material added with Pr
CN106623889A (en) * 2015-10-31 2017-05-10 杨欣睿 Fe-Ni-Nd type alloy wave-absorbing micro powder and preparation method thereof
CN106623948A (en) * 2015-10-31 2017-05-10 杨欣睿 Er-Fe-Ni alloy absorbing material

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106552945A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt-base alloys of doping Si inhales ripple micro mist and preparation method thereof
CN106552947A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt alloy of addition boron inhales ripple micro mist
CN106552946A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt alloy of addition vanadium inhales the preparation method of ripple micro mist
CN106552948A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt-base alloyss of Doped with Titanium inhale the preparation technology of ripple micropowder
CN106552933A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt-base alloyss of doping Al inhale ripple micropowder and its preparation technology
CN106552934A (en) * 2015-09-29 2017-04-05 吴涵 A kind of dysprosium cobalt alloy of addition chromium inhales ripple micropowder material
CN106552949A (en) * 2015-09-30 2017-04-05 吴涵 A kind of Dy-Co-Ga types alloy inhales ripple micropowder material and preparation method thereof
CN106607581A (en) * 2015-10-25 2017-05-03 杨欣睿 Rare earth Ce-doped alloy wave absorbing micro powder and preparing technology thereof
CN106607593A (en) * 2015-10-25 2017-05-03 杨欣睿 Fe-Ni base alloy wave absorbing micro powder added with Tb and preparation process of Fe-Ni base alloy wave absorbing micro powder
CN106607590A (en) * 2015-10-25 2017-05-03 杨欣睿 Fe-Ni-based alloy absorbing material
CN106607580A (en) * 2015-10-25 2017-05-03 杨欣睿 A rare earth-added alloy wave absorbing material
CN106607592A (en) * 2015-10-25 2017-05-03 杨欣睿 Y-doped rare earth alloy wave absorbing micro powder and preparing method thereof
CN106607591A (en) * 2015-10-25 2017-05-03 杨欣睿 Fe-Ni-based alloy absorbing material added with Pr
CN106623889A (en) * 2015-10-31 2017-05-10 杨欣睿 Fe-Ni-Nd type alloy wave-absorbing micro powder and preparation method thereof
CN106623948A (en) * 2015-10-31 2017-05-10 杨欣睿 Er-Fe-Ni alloy absorbing material
CN106334798A (en) * 2016-09-09 2017-01-18 电子科技大学 Preparation method for Fe-based nanocrystalline alloy flake micropowder
CN106334798B (en) * 2016-09-09 2019-11-15 电子科技大学 The preparation method of Fe Based Nanocrystalline Alloys sheet micro mist

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