CN102360658A - Block-shaped magnetic material and preparation method thereof - Google Patents

Block-shaped magnetic material and preparation method thereof Download PDF

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Publication number
CN102360658A
CN102360658A CN2011102795758A CN201110279575A CN102360658A CN 102360658 A CN102360658 A CN 102360658A CN 2011102795758 A CN2011102795758 A CN 2011102795758A CN 201110279575 A CN201110279575 A CN 201110279575A CN 102360658 A CN102360658 A CN 102360658A
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block
magnetic material
alloy
shaped magnetic
preparation
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简红
严密
范建江
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NINGBO ALST ELECTRICAL CO Ltd
Zhejiang University ZJU
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NINGBO ALST ELECTRICAL CO Ltd
Zhejiang University ZJU
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Abstract

The invention discloses a block-shaped magnetic material and a preparation method thereof. The general chemical molecular formula of the block-shaped magnetic material is Fe100-w-x-y-zCowRxByMz, wherein R is one or two of Nd and Pr; M is one or more of the elements Nb, Ti, Zr, Mo, Cr, V, W, Ta, Cu, Al, Zn, Ni, Ga, Ge, Sr, Si, Y, Tb, Dy, La, Ce, Hf, Sm, and Ho; and w, x, y and z are respectively atom percent of element Co, element R, element B and element M, and the atom percent of Fe is 100-w-x-y-z. The preparation method comprises the following steps: compounding various raw materials according to the alloy chemical molecular formula, and smelting to prepare mother alloy; then preparing the block-shaped magnetic material by a mould spray casting or suction casting rapid quenching process; performing heat treatment for 5-60 minutes; and optimizing alloy phase compositions and microstructures, thus obtaining the block-shaped magnetic material. The preparation method disclosed by the invention has the advantages of simple process and small energy consumption; and the block-shaped magnetic material thus obtained has the advantages of compact structure, good magnetic hardness and high corrosion-resistant property, and can be widely applied in the field of information, communication, computer, and the like.

Description

A kind of block-shaped magnetic material and preparation method thereof
Technical field
The present invention relates to magnetic material, relate in particular to a kind of block-shaped magnetic material and preparation method thereof.
Background technology
The rare earth permanent-magnetic material that with Nd-Fe-B is representative since finding the eighties in 20th century since its excellent magnetism can, developing rapidly becomes permanent magnet of new generation; And be widely used in the energy, machinery, traffic; Computer; Household electrical appliances, fields such as medical treatment, it is produced and the Application and Development degree has become one of important symbol of weighing a modern state level of economic development and overall national strength.The preparation method of traditional permanent magnet mainly contains two kinds of sintering process and mull techniques.Sintering process is to obtain magnetic through certain flouring technology, and oriented moulding in magnetic field is pressed into blank in press, and sinter molding obtains permanent magnet then.This method complex process, energy consumption is high, and can not satisfy the demand of complicated shape.Mull technique also is to obtain magnetic through certain flouring technology, with magnetic and binding agent mixed-forming, obtains permanent magnet through after the cured.Because the introducing of binding agent makes that the magnet magnetic property is diluted, so this method is unfavorable for obtaining high performance permanent magnet.In addition, traditional preparation method also is not suitable for preparing undersized block magnet, therefore is necessary to explore a kind of permanent magnet preparation method of efficient energy-saving.
In recent years, some researchers adopt copper mold spray to cast method directly to be worth cylindric, circular and flaky permanent magnet.This method be alloy spray to cast with fusion in the copper mold of certain size, directly obtain nanocrystalline permanent magnet, perhaps obtain non-crystaline amorphous metal earlier, again its heat treatment is obtained permanent magnet.It is simple that this method has technology, low cost, and easy-formation is prone to processing, compact structure, advantage such as corrosion resistance is strong.Yet because the restriction of amorphous formation ability, up to the present report is no more than 1.5mm with the magnet size that this method prepares in the document.Add and the adjusting element ratio through element in rare-earth iron series permanent-magnet alloy system in this laboratory, and adopt mould spray to cast quick quenching technique directly to make and be of a size of 0.3mm ~ 20mm, the block-shaped magnetic material of function admirable, this is most important for applying of permanent magnet.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of block-shaped magnetic material and preparation method thereof is provided.
The chemical molecular general formula of block-shaped magnetic material is Fe 100-w-x-y-zCo wR xB yM z, wherein R is one or both among Nd and the Pr, M is Nb, Ti, Zr, Mo, Cr, V, W, Ta; Cu, Al, Zn, Ni, Ga, Ge, Sr, Si, Y, Tb; Dy, La, Ce, Hf, Sm, one or more in the Ho element, w, x, y and z are respectively the Co element, the R element; B element and M elements atomic percentage, the atomic percent of Fe are 100-w-x-y-z, wherein, 0≤w≤30 at.%, 5≤x≤12 at.%,, 8≤y≤25 at.%, 0≤z≤10 at.%, remaining is Fe content.
The maximum magnetic energy product of said block-shaped magnetic material (BH) MaxBe 3 ~ 30MGOe.
Its step of the preparation method of block-shaped magnetic material is following:
Step 1: with feed metal Fe, Co, Nd, Pr, Nb, Ti, Zr, Mo, Cr, V, W, Ta, Cu, Al, Zn, Ni, Ga, Ge, Sr, Si, Y, Tb, Dy, La, Ce, Hf, Sm, Ho and FeB alloy are according to Fe 100-w-x-y-zCo wR xB yM zAlloying component according to the atomic percent weighing and the batching, with claim the repeatedly melting of target component raw material, make the uniform foundry alloy of composition;
Step 2: the Fe of step 1 acquisition 100-w-x-y-zCo wR xB yM zBroken frustillatum Fe behind the foundry alloy scale removal 100-w-x-y-zCo wR xB yM zAlloy;
Step 3: the fritter shape Fe that obtains with step 2 100-w-x-y-zCo wR xB yM zPack into lower ending opening and aperture of alloy is in the quartz ampoule of 0.4mm ~ 1mm; After vacuumizing; In cavity, charge into inert gas as protection gas, adopt the radio-frequency induction coil heating to make alloy melting, regulate electric current by little increase; Treat after the complete fusion of alloy that spray to cast or suction cast onto chilling in the mould, make block Fe 100-w-x-y-zCo wR xB yM zAlloy.
Step 4: with the Fe that obtains 100-w-x-y-zCo wR xB yM zAlloy block is annealed in vacuum environment, is heated to 500 ~ 1000 ℃ with the heating rate of 5 ~ 30 ℃/min, insulation 5 ~ 60 min, and chilling in the cold water obtains Fe then 100-w-x-y-zCo wR xB yM zBlock-shaped magnetic material.
Said block-shaped magnetic material is of a size of 0.3mm ~ 20mm.
The present invention combines heat treatment successfully to prepare the block-shaped magnetic material that is of a size of 0.3mm ~ 20mm through the mould quick quenching technique, and this method technology is simple, and energy consumption is low; Easy-formation, prepared block-shaped magnetic material compact structure, hard magnetic property is good; Decay resistance is high, has favorable industrial application prospect.
Embodiment
The chemical molecular general formula of block-shaped magnetic material is Fe 100-w-x-y-zCo wR xB yM z, wherein R is one or both among Nd and the Pr, M is Nb, Ti, Zr, Mo, Cr, V, W, Ta; Cu, Al, Zn, Ni, Ga, Ge, Sr, Si, Y, Tb; Dy, La, Ce, Hf, Sm, one or more in the Ho element, w, x, y and z are respectively the Co element, the R element; B element and M elements atomic percentage, the atomic percent of Fe are 100-w-x-y-z, wherein, 0≤w≤30 at.%, 5≤x≤12 at.%,, 8≤y≤25 at.%, 0≤z≤10 at.%, remaining is Fe content.
The maximum magnetic energy product of said block-shaped magnetic material (BH) MaxBe 3 ~ 30MGOe.
Its step of the preparation method of block-shaped magnetic material is following:
Step 1: with feed metal Fe, Co, Nd, Pr, Nb, Ti, Zr, Mo, Cr, V, W, Ta, Cu, Al, Zn, Ni, Ga, Ge, Sr, Si, Y, Tb, Dy, La, Ce, Hf, Sm, Ho and FeB alloy are according to Fe 100-w-x-y-zCo wR xB yM zAlloying component according to the atomic percent weighing and the batching, with claim the repeatedly melting of target component raw material, make the uniform foundry alloy of composition;
Step 2: the Fe of step 1 acquisition 100-w-x-y-zCo wR xB yM zBroken frustillatum Fe behind the foundry alloy scale removal 100-w-x-y-zCo wR xB yM zAlloy;
Step 3: the fritter shape Fe that obtains with step 2 100-w-x-y-zCo wR xB yM zPack into lower ending opening and aperture of alloy is in the quartz ampoule of 0.4mm ~ 1mm; After vacuumizing; In cavity, charge into inert gas as protection gas, adopt the radio-frequency induction coil heating to make alloy melting, regulate electric current by little increase; Treat after the complete fusion of alloy that spray to cast or suction cast onto chilling in the mould, make block Fe 100-w-x-y-zCo wR xB yM zAlloy.
Step 4: with the Fe that obtains 100-w-x-y-zCo wR xB yM zAlloy block is annealed in vacuum environment, is heated to 500 ~ 1000 ℃ with the heating rate of 5 ~ 30 ℃/min, insulation 5 ~ 60 min, and chilling in the cold water obtains Fe then 100-w-x-y-zCo wR xB yM zBlock-shaped magnetic material.
Said block-shaped magnetic material is of a size of 0.3mm ~ 20mm.
To combine embodiment that the present invention is done further detailed description below.
Embodiment 1: preparation Nd 7Pr 2Fe 67Nb 3B 21Block-shaped magnetic material
It is 2mm that this embodiment adopts copper mold spray to cast method to prepare diameter, and length is at the columned Nd of 1.5cm-3cm 7Pr 2Fe 67Nb 3B 21Block-shaped magnetic material.
Step 1: press atomic percent Nd 7Pr 2Fe 67Nb 3B 21Weighing purity is 99.9% Fe; Purity is 99.5% Nd; Purity is 99.5% Pr, and purity is 99.9% Nb and FeB alloy, with claim the target component raw material put into vacuum arc melting furnace; Utilize electric arc to make raw material fusing after vacuumizing, and with its melt back 5 times to obtain the uniform Nd of composition 7Pr 2Fe 67Nb 3B 21Foundry alloy.
Step 2: the Nd of step 1 acquisition 7Pr 2Fe 67Nb 3B 21Be broken into fritter behind the foundry alloy scale removal.
Step 3: the Nd that obtains with step 2 7Pr 2Fe 67Nb 3B 21Pack into lower ending opening and aperture of fritter alloy is in the quartz ampoule of 0.4mm ~ 1mm, is evacuated to 4.0 * 10 -3Behind the Pa, in the cavity of spun furnace, charge into high-purity argon gas protection, adopt the radio-frequency induction coil heating, regulate electric current by little increase, treating to spray and inject internal diameter after the complete fusion of alloy is the copper mold of 2mm, makes bulk alloy.
Step 4: with the Nd that obtains 7Pr 2Fe 67Nb 3B 21After the Vacuum Package, the heating rate with 10 ℃/min in box-annealing furnace is heated to 740 ℃ to bulk alloy in quartz ampoule, insulation 10min, chilling in 10 ~ 20 ℃ of cold water then.
Nd according to above-mentioned prepared 7Pr 2Fe 67Nb 3B 21Block-shaped magnetic material is complete amorphous at the spray to cast state, after Overheating Treatment, separate out the Hard Magnetic phase (Nd, Pr) 2Fe 14B, transmission electron microscope picture surface microstructure is tiny evenly.Magnet has good hard magnetic property, saturation magnetization M s=1.2T, coercive force H Ci=7.55KOe, magnetic energy product (BH) Max=5.6MGOe.
Embodiment 2: preparation Nd 11Fe 60Co 11Zr 3B 15Block-shaped magnetic material
It is 3mm that this embodiment adopts copper mold casting to prepare thickness, and width is 7mm, and length is at the Nd of 1.5cm-3cm sheet 11Fe 60Co 11Zr 3B 15Block-shaped magnetic material.
Step 1: press atomic percent Nd 11Fe 60Co 11Zr 3B 15Weighing purity is 99.9% Fe, and purity is 99.9% Co, and purity is 99.5% Nd; Purity is 99.9% Zr and FeB alloy; With claim the target component raw material put into vacuum arc melting furnace, utilize electric arc to make raw material fusing after vacuumizing, and melt back 5 times is to obtain the uniform Nd of composition 11Fe 60Co 11Zr 3B 15Foundry alloy.
Step 2: the Nd of step 1 acquisition 11Fe 60Co 11Zr 3B 15Be broken into fritter behind the foundry alloy spindle scale removal.
Step 3: the Nd that obtains with step 2 11Fe 60Co 11Zr 3B 15Pack into lower ending opening and aperture of fritter alloy is in the quartz ampoule of 0.4mm ~ 1mm, is evacuated to 4.0 * 10 -3Behind the Pa, in the cavity of spun furnace, charge into high-purity argon gas protection, adopt the radio-frequency induction coil heating, regulate electric current, treat to inhale after the complete fusion of alloy and cast onto in the copper mold, make the sheet alloy by little increase.
Step 4: with the Nd that obtains 11Fe 60Co 11Zr 3B 15After the Vacuum Package, the heating rate with 10 ℃/min in box-annealing furnace is heated to 730 ℃ to the sheet alloy sample in quartz ampoule, insulation 10min, chilling in 10 ~ 20 ℃ of cold water.
Nd according to above-mentioned prepared 11Fe 60Co 11Zr 3B 15Block-shaped magnetic material was complete amorphous before heat treatment, after Overheating Treatment, separated out Hard Magnetic phase Nd 2Fe 14B, transmission electron microscope picture surface microstructure is tiny evenly.Magnet has good hard magnetic property, saturation magnetization M s=1.3T, coercive force H Ci=7.12KOe, magnetic energy product (BH) Max=6.4MGOe.
Embodiment 3: preparation Nd 8Pr 1Fe 78Zr 1Ti 2B 10Block-shaped magnetic material
It is 5mm that this embodiment adopts copper mold spray to cast method to prepare external diameter, and thickness is the circular Nd of 0.5mm 8Pr 1Fe 78Zr 1Ti 2B 10Block-shaped magnetic material.
Step 1: press atomic percent Nd 8Pr 1Fe 78Zr 1Ti 2B 10Weighing purity is 99.9% Fe, and purity is 99.5% Nd, and purity is 99.9% Zr; Purity is 99.9% Ti and FeB alloy; With claim the target component raw material put into vacuum arc melting furnace, utilize electric arc to make raw material fusing after vacuumizing, and melt back 5 times is to obtain the uniform Nd of composition 8Pr 1Fe 78Zr 1Ti 2B 10Foundry alloy.
Step 2: the Nd of step 1 acquisition 8Pr 1Fe 78Zr 1Ti 2B 10Be broken into fritter behind the foundry alloy scale removal.
Step 3: the Nd that obtains with step 2 8Pr 1Fe 78Zr 1Ti 2B 10Pack into lower ending opening and aperture of fritter alloy is in the quartz ampoule of 0.4mm ~ 1mm, is evacuated to 4.0 * 10 -3Behind the Pa, in the cavity of spun furnace, charge into high-purity argon gas protection, adopt the radio-frequency induction coil heating, regulate electric current, treat to spray and injection ring-type copper mold after the complete fusion of alloy, make block alloy by little increase.
Step 4: with the Nd that obtains 8Pr 1Fe 78Zr 1Ti 2B 10After the Vacuum Package, the heating rate with 10 ℃/min in box-annealing furnace is heated to 740 ℃ to block alloy in quartz ampoule, insulation 15min, chilling in 10 ~ 20 ℃ of cold water.
Nd according to above-mentioned prepared 8Pr 1Fe 78Zr 1Ti 2B 10Block-shaped magnetic material is complete amorphous at the spray to cast state, after Overheating Treatment, separate out the Hard Magnetic phase (Nd, Pr) 2Fe 14B, transmission electron microscope picture surface microstructure is tiny evenly.Magnet has good hard magnetic property, saturation magnetization M s=1.3T, coercive force H Ci=8.79KOe, magnetic energy product (BH) Max=8.9MGOe.
Each item performance of the block-shaped magnetic material that the foregoing description obtains is shown in table 1 summary.
Table 1 Fe 100-w-x-y-zCo wR xB yM zThe performance of block-shaped magnetic material
Alloying component M s(T) M r(T) iH c(kOe) M r/M s (BH) max(MGOe)
Nd 7Pr 2Fe 67Nb 3B 21 1.2 0.7 7.55 0.58 5.6
Nd 11Fe 60Co 11Zr 3B 15 1.3 0.9 7.12 0.69 6.4
Nd 8Pr 1Fe 78Zr 1Ti 2B 10 1.3 0.9 8.79 0.69 8.9

Claims (4)

1. block-shaped magnetic material, it is characterized in that: its chemical molecular general formula is Fe 100-w-x-y-zCo wR xB yM z, wherein R is one or both among Nd and the Pr, M is Nb, Ti, Zr, Mo, Cr, V, W, Ta; Cu, Al, Zn, Ni, Ga, Ge, Sr, Si, Y, Tb; Dy, La, Ce, Hf, Sm, one or more in the Ho element, w, x, y and z are respectively the Co element, the R element; B element and M elements atomic percentage, the atomic percent of Fe are 100-w-x-y-z, wherein, 0≤w≤30 at.%, 5≤x≤12 at.%,, 8≤y≤25 at.%, 0≤z≤10 at.%, remaining is Fe content.
2. a kind of block-shaped magnetic material according to claim 1 is characterized in that: the maximum magnetic energy product of said block-shaped magnetic material (BH) MaxBe 3 ~ 30MGOe.
3. the preparation method of a block-shaped magnetic material as claimed in claim 1 is characterized in that its step is following:
Step 1: with feed metal Fe, Co, Nd, Pr, Nb, Ti, Zr, Mo, Cr, V, W, Ta, Cu, Al, Zn, Ni, Ga, Ge, Sr, Si, Y, Tb, Dy, La, Ce, Hf, Sm, Ho and FeB alloy are according to Fe 100-w-x-y-zCo wR xB yM zAlloying component according to the atomic percent weighing and the batching, with claim the repeatedly melting of target component raw material, make the uniform foundry alloy of composition;
Step 2: the Fe of step 1 acquisition 100-w-x-y-zCo wR xB yM zBroken frustillatum Fe behind the foundry alloy scale removal 100-w-x-y-zCo wR xB yM zAlloy;
Step 3: the fritter shape Fe that obtains with step 2 100-w-x-y-zCo wR xB yM zPack into lower ending opening and aperture of alloy is in the quartz ampoule of 0.4mm ~ 1mm; After vacuumizing; In cavity, charge into inert gas as protection gas, adopt the radio-frequency induction coil heating to make alloy melting, regulate electric current by little increase; Treat after the complete fusion of alloy that spray to cast or suction cast onto chilling in the mould, make block Fe 100-w-x-y-zCo wR xB yM zAlloy;
Step 4: with the Fe that obtains 100-w-x-y-zCo wR xB yM zAlloy block is annealed in vacuum environment, is heated to 500 ~ 1000 ℃ with the heating rate of 5 ~ 30 ℃/min, insulation 5 ~ 60 min, and chilling in the cold water obtains Fe then 100-w-x-y-zCo wR xB yM zBlock-shaped magnetic material.
4. the preparation method of a kind of block-shaped magnetic material according to claim 3, it is characterized in that: said block-shaped magnetic material is of a size of 0.3mm ~ 20mm.
CN2011102795758A 2011-09-20 2011-09-20 Block-shaped magnetic material and preparation method thereof Pending CN102360658A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102360702A (en) * 2011-09-20 2012-02-22 浙江大学 Simple and convenient functional magnetic material block and preparation method thereof
CN102856029A (en) * 2012-04-20 2013-01-02 漯河市三鑫稀土永磁材料有限责任公司 High (BH)max quick quenching magnetic powder and preparation method thereof
CN106856118A (en) * 2015-12-08 2017-06-16 北京中科三环高技术股份有限公司 The thinning method and bonded permanent magnet of nanocrystalline fast quenching rare-earth permanent-magnet material and its crystallite dimension
CN108630369A (en) * 2018-06-19 2018-10-09 江苏江淮磁业有限公司 A kind of neodymium cerium Fe-Mn magnetism material preparation method based on cerium

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Publication number Priority date Publication date Assignee Title
CN101117693A (en) * 2007-09-13 2008-02-06 上海大学 FeZrNdYB nano block alloy having hard magnetism and method for preparing same
CN101844219A (en) * 2010-04-22 2010-09-29 宁波大学 A kind of preparation method of block nanometer composite R-Fe-B-M permanent-magnet material
CN101886233A (en) * 2010-06-29 2010-11-17 上海大学 Fe base block alloy with hard magnetic property and preparation method thereof
CN102360702A (en) * 2011-09-20 2012-02-22 浙江大学 Simple and convenient functional magnetic material block and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101117693A (en) * 2007-09-13 2008-02-06 上海大学 FeZrNdYB nano block alloy having hard magnetism and method for preparing same
CN101844219A (en) * 2010-04-22 2010-09-29 宁波大学 A kind of preparation method of block nanometer composite R-Fe-B-M permanent-magnet material
CN101886233A (en) * 2010-06-29 2010-11-17 上海大学 Fe base block alloy with hard magnetic property and preparation method thereof
CN102360702A (en) * 2011-09-20 2012-02-22 浙江大学 Simple and convenient functional magnetic material block and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102360702A (en) * 2011-09-20 2012-02-22 浙江大学 Simple and convenient functional magnetic material block and preparation method thereof
CN102856029A (en) * 2012-04-20 2013-01-02 漯河市三鑫稀土永磁材料有限责任公司 High (BH)max quick quenching magnetic powder and preparation method thereof
CN106856118A (en) * 2015-12-08 2017-06-16 北京中科三环高技术股份有限公司 The thinning method and bonded permanent magnet of nanocrystalline fast quenching rare-earth permanent-magnet material and its crystallite dimension
CN108630369A (en) * 2018-06-19 2018-10-09 江苏江淮磁业有限公司 A kind of neodymium cerium Fe-Mn magnetism material preparation method based on cerium

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Application publication date: 20120222