CN103317145A - Method for preparing samarium cobalt magnetic powder by chemical method - Google Patents

Method for preparing samarium cobalt magnetic powder by chemical method Download PDF

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CN103317145A
CN103317145A CN2013102865302A CN201310286530A CN103317145A CN 103317145 A CN103317145 A CN 103317145A CN 2013102865302 A CN2013102865302 A CN 2013102865302A CN 201310286530 A CN201310286530 A CN 201310286530A CN 103317145 A CN103317145 A CN 103317145A
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powder
samarium
magnetic powder
nitrate
cobalt magnetic
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CN103317145B (en
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于濂清
王清清
韩雪
徐东
鲁文博
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China University of Petroleum East China
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China University of Petroleum East China
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Abstract

The invention discloses a method for preparing samarium cobalt magnetic powder by the chemical method. The method includes the following steps: (1) dissolving samarium nitrate, cobalt nitrate, nitrate of metal M and citric acid into water, (2) carrying out heating and stirring to obtain sol, (3) drying the sol to form gel powder, (4) carrying out heat treatment in the air to obtain black powder, (5) evenly mixing the black powder with calcium powder, and carrying out restoration heat treatment in a vacuum tubular furnace to obtain the samarium cobalt magnetic powder. The sizes of particles of the magnetic powder prepared by the method are 0.01 micrometer to 50 micrometers and controllable, the particle size distribution is narrow, and the magnetic powder can be used as sintering samarium cobalt magnetic powder and can also be used as bonding samarium cobalt magnetic powder.

Description

Chemical method prepares the method for samarium-cobalt magnetic powder
Technical field
The present invention relates to the method that a kind of chemical method prepares samarium-cobalt magnetic powder.
Background technology
Rare earth SmCo permanent magnet is widely used in the industry such as electronics, instrument and space flight, and it has unique magnetic property, behind replacement ferrite or the AlNiCo, and the energy energy savings, reduced volume, weight reduction improves limit magnetic flux density.Samarium-cobalt permanent-magnetic material is mainly used in the permanent magnetism small and special electric machine, under the particular surroundings such as high temperature, high vacuum, the application of samarium cobalt permanent magnet motor is occupied an leading position, small and light with the motor that samarium-cobalt magnet makes, accurately, easy to control again, and material cost is feasible, can be used for the lathe of requirement Precision Machining control.In the information industry field, all need annular, rectangle, polygonal samarium cobalt permanent magnet body in the electronic technology communication, the in addition application in the magnet ring electro-acoustic element in the GSM third generation mobile phone, the electro-acoustic elements such as high-grade microphone, audiphone, sound pick-up, Microspeaker all be unable to do without the high-performance samarium cobalt permanent magnet.
At present, main SmCo based permanent magnetic material comprises SmCo 5, Sm 2Co 17, SmCo 7The compound of three types.SmCo 5The type magnet has higher magnetic property, but contains the strategy metal Co rare up to the costliness of 67wt.% (percentage by weight) and the rare earth metal Sm of 33wt.%, and cost is very high, and application is limited by very large.Sm 2Co 17Type permanent magnetism has larger saturation magnetization, and good monadic magnetocrystalline anisotropy (easily c-axis) and higher Curie temperature are a kind of potential desirable permanent-magnet materials.But its magnetocrystalline anisotropy field is lower, is difficult to become practical magnet.In order to improve magnetic property, people are developed Sm from two aspects 2Co 17The type permanent-magnet material adds on the one hand the element such as Mn, Cr and develops high performance permanent-magnet material; The permanent-magnet material in Sm-Co-Cu-Fe series on the other hand.
The granularity of SmCo powder is the key factor that affects SmCo base magnet sintering quality and magnetic property, and the magnet crystallite dimension that traditional melting, powder process, sintering, solid process of smelting obtain is very large, and is unfavorable to magnetic property.The SmCo magnetic powder particles size that the present invention adopts sol-gal process to prepare is controlled at 0.01-50 μ m, narrow particle size distribution, and this Magnaglo can be used as the sintered samarium cobalt magnetic, also can be used as the bonding samarium-cobalt magnetic powder.
Summary of the invention
The purpose of this invention is to provide the method that a kind of chemical method prepares samarium-cobalt magnetic powder.
Its step is:
1) nitrate with samaric nitrate, cobalt nitrate, metal M is dissolved in the deionized water, wherein the ratio of element samarium, cobalt, metal M is pressed the composition proportion interpolation of samarium-cobalt magnetic powder, nitrate concentration is controlled at 0.5-10mol/L, then add citric acid, the mol ratio of citric acid and nitrate anion is 1:(0.1-10), uniform stirring mixes;
2) above-mentioned mixed solution is heated to 50-95 ℃ after, stirred 0.5-10 hour, be cooled to 10-20 ℃, obtain colloidal sol;
3) colloidal sol is put into baking oven, temperature is 70-120 ℃, dries 0.5-10 hour, until form gel powder;
4) then with above-mentioned gel powder in air 400-1000 ℃ heat treatment 1-4 hour, obtain black powder;
5) black powder is evenly mixed with calcium powder, the shared mass fraction of calcium powder is 5-40%, carries out heat of reduction and processed 0.5-4 hour in vacuum tube furnace, and temperature is 600-1000 ℃, then acetic acid and the water with 1-10% cleans 3-5 time repeatedly, obtains the SmCo powder after the vacuum drying.
The composition proportion of described samarium-cobalt magnetic powder is Sm xCo yM 100-x-y(mass percent), wherein 2≤x≤50,30≤y≤98.
Described metal M is in Dy, Tb, Nb, Fe, Ga, Zr, Mn, Cr, Ti, Ni, Al, Gd, the Cu element one or more.
Described SmCo Magnaglo size is at 0.01-50 μ m.
Described SmCo powder can be used as the sintered samarium cobalt magnetic, also can be used as the bonding samarium-cobalt magnetic powder.
The magnetic powder particles size that the present invention prepares is controlled, narrow particle size distribution, and this Magnaglo can be used as the sintered samarium cobalt magnetic, also can be used as the bonding samarium-cobalt magnetic powder.
The specific embodiment
The SmCo magnetic powder particles size that the present invention adopts sol-gal process to prepare is controlled at 0.01-50 μ m, narrow particle size distribution, and this Magnaglo can be used as the sintered samarium cobalt magnetic, also can be used as the bonding samarium-cobalt magnetic powder.
Concrete steps of the present invention are as follows:
1) nitrate with samaric nitrate, cobalt nitrate, metal M is dissolved in the deionized water, wherein the ratio of element samarium, cobalt, metal M is pressed the composition proportion interpolation of samarium-cobalt magnetic powder, nitrate concentration is at 0.5-10mol/L, then add citric acid, the mol ratio of citric acid and nitrate anion is 1:(0.1-10), uniform stirring mixes, and the composition proportion of samarium-cobalt magnetic powder is Sm xCo yM 100-x-y(mass percent), 2≤x≤50,30≤y≤98 wherein, metal M is in Dy, Tb, Nb, Fe, Ga, Zr, Mn, Cr, Ti, Ni, Al, Gd, the Cu element one or more;
2) above-mentioned mixed solution is heated to 50-95 ℃ after, stirred 0.5-10 hour, be cooled to 10-20 ℃, obtain colloidal sol;
3) colloidal sol is put into baking oven, temperature is 70-120 ℃, dries 0.5-10 hour, until form gel powder;
4) then with above-mentioned gel powder in air 400-1000 ℃ heat treatment 1-4 hour, obtain black powder;
5) black powder is evenly mixed with calcium powder, the shared mass fraction of calcium powder is 5-40%, carrying out heat of reduction in vacuum tube furnace processed 0.5-4 hour, temperature is 600-1000 ℃, then acetic acid and the water with 1-10% cleans 3-5 time repeatedly, obtains the SmCo powder size after the vacuum drying at 0.01-50 μ m.
Embodiment 1:
1) samaric nitrate, cobalt nitrate, ferric nitrate are dissolved in the deionized water by the composition proportion of samarium-cobalt magnetic powder, then nitrate concentration adds citric acid at 1mol/L, and the mol ratio of citric acid and nitrate anion is 1:2, uniform stirring mixes, and the composition proportion of samarium-cobalt magnetic powder is Sm 45Co 54.5Fe 0.5(mass percent);
2) above-mentioned mixed solution is heated to 90 ℃ after, stirred 5 hours, be cooled to 20 ℃, obtain colloidal sol;
3) colloidal sol is put into baking oven, temperature is 120 ℃, dries 5 hours, until form gel powder;
4) then with the 600 ℃ of heat treatment 1 hour in air of above-mentioned gel powder, obtain black powder;
5) black powder is evenly mixed with calcium powder, the shared mass fraction of calcium powder is 40%, carries out heat of reduction and processed 1 hour in vacuum tube furnace, and temperature is 700 ℃, then repeatedly clean 5 times with 4% acetic acid and water, obtain the SmCo powder size after the vacuum drying at 0.03 μ m.
The magnetic powder particles size that the present invention prepares is controlled, narrow particle size distribution, and maximum magnetic energy product is 9.4 * 10 6High oersted, this Magnaglo can be used as the sintered samarium cobalt magnetic, also can be used as the bonding samarium-cobalt magnetic powder.
Embodiment 2:
1) samaric nitrate, cobalt nitrate, manganese nitrate, chromic nitrate are dissolved in the deionized water by the composition proportion of samarium-cobalt magnetic powder, then nitrate concentration adds citric acid at 3mol/L, and the mol ratio of citric acid and nitrate anion is 1:0.5, uniform stirring mixes, and the composition proportion of samarium-cobalt magnetic powder is Sm 40Co 58Mn 1Cr 1(mass percent);
2) above-mentioned mixed solution is heated to 60 ℃ after, stirred 0.5 hour, be cooled to 20 ℃, obtain colloidal sol;
3) colloidal sol is put into baking oven, temperature is 100 ℃, dries 6 hours, until form gel powder;
4) then with the 500 ℃ of heat treatment 2 hours in air of above-mentioned gel powder, obtain black powder;
5) black powder is evenly mixed with calcium powder, the shared mass fraction of calcium powder is 30%, carries out heat of reduction and processed 1 hour in vacuum tube furnace, and temperature is 950 ℃, then repeatedly clean 3 times with 3% acetic acid and water, obtain the SmCo powder size after the vacuum drying at 5 μ m.
The magnetic powder particles size that the present invention prepares is controlled, narrow particle size distribution, and maximum magnetic energy product is 1.8 * 10 5High oersted, this Magnaglo can be used as the sintered samarium cobalt magnetic, also can be used as the bonding samarium-cobalt magnetic powder.
Embodiment 3:
1) samaric nitrate, cobalt nitrate, ferric nitrate, copper nitrate, zirconium nitrate are dissolved in the deionized water by the composition proportion of samarium-cobalt magnetic powder, then nitrate concentration adds citric acid at 3mol/L, and the mol ratio of citric acid and nitrate anion is 1:3, uniform stirring mixes, and the composition proportion of samarium-cobalt magnetic powder is Sm 45Co 35Fe 18Cu 1.5Zr 0.5(mass percent);
2) above-mentioned mixed solution is heated to 80 ℃ after, stirred 5 hours, be cooled to 20 ℃, obtain colloidal sol;
3) colloidal sol is put into baking oven, temperature is 90 ℃, dries 8 hours, until form gel powder;
4) then with the 550 ℃ of heat treatment 1 hour in air of above-mentioned gel powder, obtain black powder;
5) black powder is evenly mixed with calcium powder, the shared mass fraction of calcium powder is 20%, carries out heat of reduction and processed 3 hours in vacuum tube furnace, and temperature is 850 ℃, then repeatedly clean 3 times with 3% acetic acid and water, obtain the SmCo powder size after the vacuum drying at 0.8 μ m.
The magnetic powder particles size that the present invention prepares is controlled, narrow particle size distribution, and maximum magnetic energy product is 4.5 * 10 6High oersted, this Magnaglo can be used as the sintered samarium cobalt magnetic, also can be used as the bonding samarium-cobalt magnetic powder.
Embodiment 4:
1) samaric nitrate, cobalt nitrate, ferric nitrate, Titanium Nitrate are dissolved in the deionized water by the composition proportion of samarium-cobalt magnetic powder, then nitrate concentration adds citric acid at 3mol/L, and the mol ratio of citric acid and nitrate anion is 1:0.8, uniform stirring mixes, and the composition proportion of samarium-cobalt magnetic powder is Sm 40Co 48Fe 10Ti 2(mass percent);
2) above-mentioned mixed solution is heated to 70 ℃ after, stirred 0.5 hour, be cooled to 20 ℃, obtain colloidal sol;
3) colloidal sol is put into baking oven, temperature is 90 ℃, dries 4 hours, until form gel powder;
4) then with the 800 ℃ of heat treatment 3 hours in air of above-mentioned gel powder, obtain black powder;
5) black powder is evenly mixed with calcium powder, the shared mass fraction of calcium powder is 34%, carries out heat of reduction and processed 2.5 hours in vacuum tube furnace, and temperature is 850 ℃, then repeatedly clean 3 times with 3% acetic acid and water, obtain the SmCo powder size after the vacuum drying at 1 μ m.
The magnetic powder particles size that the present invention prepares is controlled, narrow particle size distribution, and maximum magnetic energy product is 7.8 * 10 5High oersted, this Magnaglo can be used as the sintered samarium cobalt magnetic, also can be used as the bonding samarium-cobalt magnetic powder.

Claims (5)

1. a chemical method prepares the method for samarium-cobalt magnetic powder, it is characterized in that its step is:
1) nitrate with samaric nitrate, cobalt nitrate, metal M is dissolved in the deionized water, wherein the ratio of element samarium, cobalt, metal M is pressed the composition proportion interpolation of samarium-cobalt magnetic powder, nitrate concentration is controlled at 0.5-10mol/L, then add citric acid, the mol ratio of citric acid and nitrate anion is 1:(0.1-10), uniform stirring mixes;
2) above-mentioned mixed solution is heated to 50-95 ℃ after, stirred 0.5-10 hour, be cooled to 10-20 ℃, obtain colloidal sol;
3) colloidal sol is put into baking oven, temperature is 70-120 ℃, dries 0.5-10 hour, until form gel powder;
4) then with above-mentioned gel powder in air 400-1000 ℃ heat treatment 1-4 hour, obtain black powder;
5) black powder is evenly mixed with calcium powder, the shared mass fraction of calcium powder is 5-40%, carries out heat of reduction and processed 0.5-4 hour in vacuum tube furnace, and temperature is 600-1000 ℃, then acetic acid and the water with 1-10% cleans 3-5 time repeatedly, obtains the SmCo powder after the vacuum drying.
2. chemical method according to claim 1 prepares the method for samarium-cobalt magnetic powder, and the composition proportion that it is characterized in that described samarium-cobalt magnetic powder is Sm xCo yM 100-x-y(mass percent), wherein 2≤x≤50,30≤y≤98.
3. chemical method according to claim 1 prepares the method for samarium-cobalt magnetic powder, it is characterized in that described metal M is in Dy, Tb, Nb, Fe, Ga, Zr, Mn, Cr, Ti, Ni, Al, Gd, the Cu element one or more.
4. chemical method according to claim 1 prepares the method for samarium-cobalt magnetic powder, it is characterized in that described SmCo Magnaglo size is at 0.01-50 μ m.
5. chemical method according to claim 1 prepares the method for samarium-cobalt magnetic powder, it is characterized in that described SmCo powder can be used as the sintered samarium cobalt magnetic, also can be used as the bonding samarium-cobalt magnetic powder.
CN201310286530.2A 2013-07-09 2013-07-09 Chemical method prepares the method for samarium-cobalt magnetic powder Active CN103317145B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104157385A (en) * 2014-03-15 2014-11-19 南通万宝实业有限公司 High-coercivity samarium cobalt based permanent magnet material preparation method
CN104319046A (en) * 2014-10-11 2015-01-28 宁波科星材料科技有限公司 Samarium cobalt permanent magnet material
CN108526489A (en) * 2018-05-08 2018-09-14 重庆科技学院 Sol-gel method prepares the method and product of Sm-Co nano particles
CN109550973A (en) * 2019-01-29 2019-04-02 重庆科技学院 A kind of preparation method, magnetic powder and the magnet of AlNiCo/SmCo composite magnetic powder
CN110373591A (en) * 2019-08-01 2019-10-25 苏州航大新材料科技有限公司 A kind of magnetic material SmCo iron copper zirconium alloy and preparation method thereof

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CN102651263A (en) * 2012-05-24 2012-08-29 宁波科星材料科技有限公司 Preparation method of samarium-cobalt (SmCo) system sintered materials
CN103182514A (en) * 2013-04-11 2013-07-03 中国石油大学(华东) Method for preparing neodymium iron boron magnetic powder by self-propagating combustion

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104157385A (en) * 2014-03-15 2014-11-19 南通万宝实业有限公司 High-coercivity samarium cobalt based permanent magnet material preparation method
CN104319046A (en) * 2014-10-11 2015-01-28 宁波科星材料科技有限公司 Samarium cobalt permanent magnet material
CN104319046B (en) * 2014-10-11 2017-07-07 宁波科星材料科技有限公司 A kind of samarium-cobalt permanent-magnetic material
CN108526489A (en) * 2018-05-08 2018-09-14 重庆科技学院 Sol-gel method prepares the method and product of Sm-Co nano particles
CN109550973A (en) * 2019-01-29 2019-04-02 重庆科技学院 A kind of preparation method, magnetic powder and the magnet of AlNiCo/SmCo composite magnetic powder
CN109550973B (en) * 2019-01-29 2021-12-24 重庆科技学院 Preparation method of AlNiCo/SmCo composite magnetic powder, magnetic powder and magnet
CN110373591A (en) * 2019-08-01 2019-10-25 苏州航大新材料科技有限公司 A kind of magnetic material SmCo iron copper zirconium alloy and preparation method thereof

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