CN104942299A - Rare earth and iron-based wave-absorbing micro powder preparation method - Google Patents
Rare earth and iron-based wave-absorbing micro powder preparation method Download PDFInfo
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- CN104942299A CN104942299A CN201510245676.1A CN201510245676A CN104942299A CN 104942299 A CN104942299 A CN 104942299A CN 201510245676 A CN201510245676 A CN 201510245676A CN 104942299 A CN104942299 A CN 104942299A
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Abstract
The invention provides a Fe-Nd-Gd alloy wave-absorbing micro powder and a preparation method thereof. According to the method, metal Fe, Nd and Gd serve as raw materials and are mixed according to the atom proportion of Fe17Nd2-xGdx (0.2<=x<=1.0), wave-absorbing alloy is prepared through the operation of smelting, vacuum sealing, homogenizing, quenching and the like, then the alloy is primarily smashed mechanically and then ball-milled through a planetary ball mill under the gasoline environment protection condition, the powder is collected and dried after ball milling, and the wave-absorbing micro powder is obtained.
Description
Technical field
The present invention relates to the preparation method that a kind of rare earth-iron base inhales ripple micro mist, particularly the preparation method of ripple micro mist inhaled by the ferrous alloy of a kind of adulterate Nd, Gd, belongs to field of functional materials.
Background technology
Along with the development with anti-stealth technology stealthy in military affairs, stealth material is constantly developed, and research and development electromagnetic wave absorption material is then one of main effective way realizing the stealthy and electronic product countermeasure techniques of modern weapons equipment.In life, widely using of mobile communication, electronic device, while it brings convenience, also can cause radiation hazradial bundle to us.Electromagnetic wave absorption material also known as stealth material, as a kind of can the functional material of electromagnetic wave absorption, its effect is that external electromagnetic wave energy is converted to other forms of energy, reduces reflection intensity of wave, reaches stealthy or jamproof effect.
Absorbing material not only will have good absorbing property, also should have little thickness and surface density, good mechanical property and environment resistant performance.Absorbing material has reached tens kinds more than, in numerous absorbing material, electromagnetic wave absorbing material accounts for critical role, can be widely used in the measurement etc. of the characteristic impedance degrees of coupling such as the interference of electronic equipment, radar, aircraft and satellite with the microwave dark room that magnetizing mediums absorbing material makes; In addition magnetizing mediums absorbing material is improving compatibility that is airborne, Shipborne Radar Equipment, makes the aspect Yi You broad space such as overall performance raising.Electromagnetic wave absorbing material mainly comprises ferrite, super-fine metal powder, polycrystalline iron fiber, alloy powder etc.Ferrite has lower dielectric constant, 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 hystersis loss, eddy-current loss electromagnetic 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.Fe base alloy is widely studied with the absorbing property of excellence, although obtain certain achievement, but still there is shortcomings such as inhaling ripple frequency band is narrower, low-frequency range poor performance.Rare earth element be a class have the element of not paired 4f electronics that shields by outermost electron, thus their atom and ion have special electromagnetic performance.A certain amount of rare earth element is added in ferrous alloy, the frequency range of absorbing material absworption peak can be regulated, the coupling requirement of alloy can be regulated simultaneously, improve absorbing property.The present invention, by Nd, Gd being added in Fe base alloy, prepares a kind of alloy powder with excellent absorbing property.
Summary of the invention
The invention provides a kind of Fe-Nd-Gd alloy and inhale ripple micro mist and preparation method thereof, the method is carried out as follows:
(1) be greater than Fe, Nd, Gd metal of more than 99.5% for raw material, by Fe with purity
17nd
2-xgd
xthe atomic ratio batching of (0.2≤X≤1.0);
(2) the above-mentioned component materials for preparing is carried out alloy melting, melting more than 3 times with vacuum arc furnace ignition;
(3) take out melted alloy pig, load in quartz glass tube, be filled with argon gas as protective gas, and tube sealing sealing;
(4), in glass tube encroached water, check it whether to seal completely;
(5) again glass tube is put into annealing furnace, carry out homogenizing annealing process;
(6) annealing terminates rear taking-up sample, quenches;
(7) break glass tube, the sample in take-off pipe after quenching;
(8) sample grinding pot is carried out machinery tentatively to pulverize, be crushed to a certain degree, collect powder pulverized powder;
(9) the powder of collection is poured in ball grinder, under the protection of gasoline, carry out ball milling with planetary ball mill;
(10) after ball milling a period of time, alloy powder take out dry, a kind of Fe-Nd-Gd alloy powder absorbing material.
Preferentially, step (1) in, be Fe according to atomic ratio
17nd
2-xgd
x(0.5≤X≤0.7) prepares burden.
Preferentially, step (5) in, annealing temperature controls at 500-700 DEG C, and annealing time is 12-15 days.
Preferentially, step (9) in, ratio of grinding media to material is 15:1, and planetary ball mill speeds control 200-300 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) this preparation method's technique is simple;
(2) the alloy powder prepared inhales ripple bandwidth, and low frequency performance is good.
Detailed description of the invention
Embodiment one:
Fe, Nd, Gd metal of more than 99.5% is greater than for raw material, by Fe with purity
17nd
1.5gd
0.5ingredient composition 6g, with vacuum arc furnace ignition, the above-mentioned component materials for preparing is carried out alloy melting, melting more than 3 times, take out melted alloy pig, loaded in quartz glass tube, be filled with argon gas as protective gas, tube sealing seals, the quartz glass tube of sealing is put into its sealing of built for in-water survey, after guaranteeing sealing completely, drain away the water, again glass tube is put into the annealing furnace of 500 DEG C, carry out homogenizing annealing process, anneal 15 days, annealing terminates rear taking-up sample and puts into mixture of ice and water to quench, take out after fully cooling and smash glass tube, then alloy sample superficial layer is polished off, with mortar tank, sample is carried out machinery tentatively to pulverize, be crushed to a certain degree, collect powder pulverized powder, again powder is poured in ball grinder, under the protection of gasoline, ball milling is carried out with planetary ball mill, ball material mass ratio is 15:1, rotating speed is 200 r/min.After ball milling 70 h, gasoline is poured out, take out sample powder, dry, can obtain and inhale ripple micro mist for a kind of Fe-Nd-Gd alloy.
Embodiment two:
Fe, Nd, Gd metal of more than 99.5% is greater than for raw material, by Fe with purity
17nd
1.4gd
0.6ingredient composition 6g, with vacuum arc furnace ignition, the above-mentioned component materials for preparing is carried out alloy melting, melting more than 3 times, take out melted alloy pig, loaded in quartz glass tube, be filled with argon gas as protective gas, tube sealing seals, the quartz glass tube of sealing is put into its sealing of built for in-water survey, after guaranteeing sealing completely, drain away the water, again glass tube is put into the annealing furnace of 600 DEG C, carry out homogenizing annealing process, anneal 13 days, annealing terminates rear taking-up sample and puts into mixture of ice and water to quench, take out after fully cooling and smash glass tube, then alloy sample superficial layer is polished off, with mortar tank, sample is carried out machinery tentatively to pulverize, be crushed to a certain degree, collect powder pulverized powder, again powder is poured in ball grinder, under the protection of gasoline, ball milling is carried out with planetary ball mill, ball material mass ratio is 15:1, rotating speed is 250 r/min.After ball milling 60 h, gasoline is poured out, take out sample powder, dry, can obtain and inhale ripple micro mist for a kind of Fe-Nd-Gd alloy.
Embodiment three:
Fe, Nd, Gd metal of more than 99.5% is greater than for raw material, by Fe with purity
17nd
1.3gd
0.7ingredient composition 6g, with vacuum arc furnace ignition, the above-mentioned component materials for preparing is carried out alloy melting, melting more than 3 times, take out melted alloy pig, loaded in quartz glass tube, be filled with argon gas as protective gas, tube sealing seals, the quartz glass tube of sealing is put into its sealing of built for in-water survey, after guaranteeing sealing completely, drain away the water, again glass tube is put into the annealing furnace of 700 DEG C, carry out homogenizing annealing process, anneal 12 days, annealing terminates rear taking-up sample and puts into mixture of ice and water to quench, take out after fully cooling and smash glass tube, then alloy sample superficial layer is polished off, with mortar tank, sample is carried out machinery tentatively to pulverize, be crushed to a certain degree, collect powder pulverized powder, again powder is poured in ball grinder, under the protection of gasoline, ball milling is carried out with planetary ball mill, ball material mass ratio is 15:1, rotating speed is 300 r/min.After ball milling 50 h, gasoline is poured out, take out sample powder, dry, can obtain and inhale ripple micro mist for a kind of Fe-Nd-Gd alloy.
Claims (5)
1. a preparation method for ripple micro mist inhaled by Fe-Nd-Gd alloy, and it is characterized in that, the method comprises the steps:
(1) be greater than Fe, Nd, Gd metal of more than 99.5% for raw material, by Fe with purity
17nd
2-xgd
xthe atomic ratio batching of (0.2≤X≤1.0);
(2) the above-mentioned component materials for preparing is carried out alloy melting, melting more than 3 times with vacuum arc furnace ignition;
(3) take out melted alloy pig, load in quartz glass tube, be filled with argon gas as protective gas, and tube sealing sealing;
(4), in glass tube encroached water, check it whether to seal completely;
(5) again glass tube is put into annealing furnace, carry out homogenizing annealing process;
(6) annealing terminates rear taking-up sample, quenches;
(7) break glass tube, the sample in take-off pipe after quenching;
(8) sample grinding pot is carried out machinery tentatively to pulverize, be crushed to a certain degree, collect powder pulverized powder;
(9) the powder of collection is poured in ball grinder, under the protection of gasoline, carry out ball milling with planetary ball mill;
(10) after ball milling a period of time, alloy powder take out dry, a kind of Fe-Nd-Gd alloy powder absorbing material.
2. the preparation method of ripple micro mist inhaled by a kind of Fe-Nd-Gd alloy according to claim 1, it is characterized in that, step (1) in, Fe
17nd
2-xgd
xalloy atom ratio is 0.5≤X≤0.7.
3. the preparation method of ripple micro mist inhaled by a kind of Fe-Nd-Gd alloy according to claim 1, and it is characterized in that, annealing temperature controls at 500-700 DEG C, and annealing time is 12-15 days.
4. the preparation method of ripple micro mist inhaled by a kind of Fe-Nd-Gd alloy according to claim 1, and it is characterized in that, ratio of grinding media to material is 15:1, and planetary ball mill speeds control 200-300 r/min runs.
5. the preparation method of ripple micro mist inhaled by a kind of Fe-Nd-Gd alloy according to claim 1, and it is characterized in that, the time of carrying out ball milling with planetary ball mill is 50-70h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114621729A (en) * | 2022-03-03 | 2022-06-14 | 北矿磁材（阜阳）有限公司 | Preparation method of metal iron-based composite wave-absorbing material |
Citations (4)
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|---|---|---|---|---|
| CN101203127A (en) * | 2007-07-09 | 2008-06-18 | 四川大学 | Rare earth Fe basis suction wave material and method for making the same |
| CN101886214A (en) * | 2010-07-16 | 2010-11-17 | 兰州大学 | Electromagnetic wave absorbing material |
| CN104388818A (en) * | 2014-11-14 | 2015-03-04 | 桂林电子科技大学 | ErFeV magnetic wave-absorbing material and preparation method thereof |
| CN104451264A (en) * | 2014-12-09 | 2015-03-25 | 桂林电子科技大学 | Laceni magnetic wave absorbing material and preparation method thereof |
-
2015
- 2015-05-15 CN CN201510245676.1A patent/CN104942299A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101203127A (en) * | 2007-07-09 | 2008-06-18 | 四川大学 | Rare earth Fe basis suction wave material and method for making the same |
| CN101886214A (en) * | 2010-07-16 | 2010-11-17 | 兰州大学 | Electromagnetic wave absorbing material |
| CN104388818A (en) * | 2014-11-14 | 2015-03-04 | 桂林电子科技大学 | ErFeV magnetic wave-absorbing material and preparation method thereof |
| CN104451264A (en) * | 2014-12-09 | 2015-03-25 | 桂林电子科技大学 | Laceni magnetic wave absorbing material and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 成丽春等: "高能球磨工艺对Nd-Fe-Cr 合金吸波性能的影响", 《电子元件与材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114621729A (en) * | 2022-03-03 | 2022-06-14 | 北矿磁材（阜阳）有限公司 | Preparation method of metal iron-based composite wave-absorbing material |
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