CN101599332A - The method for preparing magnetic material of rare-earth permanent magnet ferrite - Google Patents
The method for preparing magnetic material of rare-earth permanent magnet ferrite Download PDFInfo
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- CN101599332A CN101599332A CNA2009100497437A CN200910049743A CN101599332A CN 101599332 A CN101599332 A CN 101599332A CN A2009100497437 A CNA2009100497437 A CN A2009100497437A CN 200910049743 A CN200910049743 A CN 200910049743A CN 101599332 A CN101599332 A CN 101599332A
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Abstract
The invention discloses a kind of method for preparing magnetic material of rare-earth permanent magnet ferrite, be to be major ingredient, by adding auxiliary agent, preparing the high-performance rare-earth permanent-magnetic ferrite magnetic material through wet ball grinding, the moulding of magnetizing, high temperature sintering again with the ferrite prefiring material that contains strontium or barium.The present invention is rich in the rare earth ore concentrate powder of lanthanum by interpolation or is rich in carbonate mixture that lanthanum rare earth ore concentrate powder extracts and substitutes and conventionally add the pure rare earth oxide or pure rare earth hydroxide has utilized the improvement of the lanthanum element in the rare earth to the ferrite magnetic characteristic, cerium substitutes cobalt oxide and improves its coercive force, and material parts such as iron, silicon, calcium and aluminium substitute the non rear earth oxide auxiliary agent that must add.Utilize the prepared permanent-magnet ferrite magnetic characteristic of the inventive method to be: Br 〉=390mT, Hcj 〉=250kA/m, BH
(MAX)〉=25kJ/m
3The present invention can make full use of China and be rich in lanthanum rare earth resources advantage, reduces production cost of ferrite.
Description
Technical field
The present invention relates to a kind of method for preparing the permanent-magnet ferrite magnetic material of Magnetoplumbate-type crystal structure, relate to a kind of method for preparing the high-performance rare-earth permanent-magnetic ferrite magnetic material by the interpolation rare earth in particular.
Background technology
Looking back the production of magnetic material can find: late 1960s is that main body is produced the magnetic material product with aluminium-nickel-cobalt, progressively transfers to after the seventies based on ferrite, has deeply developed the high-performance rare-earth magnetic material today again.Along with the development of the miniaturization of electronic equipment, lightness, slimming technology, volume, weight, the performance of permanent-magnet ferrite device there is more and more higher requirement.Particularly the develop rapidly of automobile, motorcycle, microcomputer industry has stimulated the demand to permanent-magnet ferrite.Medium-to-high grade in recent years market constantly enlarges, and demand constantly increases.According to statistics: global magnetic material gross output value estimation increased about 1.7 times in average per 10 years, and the output value of ferrite magnetic material in 1999 accounts for more than 50% of the global gross output value.For improving the magnetic characteristic of permanent-magnet ferrite, carry out energetically in recent years and rear-earth-dopedly improve the research of permanent-magnet ferrite performance and entered industrialization.Because rare earth permanent-magnetic material is the present known the highest a kind of permanent magnetic material of combination property, it is higher more than 100 times than the magnetic property of the magnet steel that 19th-century uses, than ferrite, aluminium nickel cobalt superior performance many, also double than the magnetic property of the platinum cobalt alloy of costliness.Because the use of rare earth permanent-magnetic material has not only promoted the permanent magnetism device to develop to miniaturization, improve the performance of product, and impelled the generation of some particular device, so rare earth permanent-magnetic material one occurs, cause the very big attention of various countries immediately, develop very rapid.Chinese invention patent as Hitachi Metal Co., Ltd.'s application, publication number: CN1253657A, time of disclosure: on May 17th, 2000, name is called " ferrite and production method thereof " and provides a kind of based on strontium or barium ferrite pre-sintered material, and the acting in conjunction of adding pure light lanthana or pure zirconia lanthanum and cobalt oxide by secondary prepares the method for high remanent magnetism and coercive force through ultra-fine grinding, wet moulding and high temperature sintering.Its molecular formula is: (A
1-xR
x) On (Fe
1-yM
y)
2O
3, wherein A represents strontium or barium atom, and R represents at least a Rare Earth Lanthanum atom, and M represents cobalt, manganese, nickel and zinc atom.Molecular structure is the Magnetoplumbate-type crystal, and the prepared ferrite magnetic characteristic is: remanent magnetism is that 0.41T, coercive force are 235kA/m.The principal character of this patent of invention is: add the acting in conjunction of pure light lanthana or pure zirconia lanthanum and cobalt oxide by secondary, thereby improve the method for ferrite remanent magnetism and coercive force.
The Chinese invention patent of Beikuan Magnetic-material Science ﹠ Technology Co., Ltd.'s application, publication number: CN1414575A, time of disclosure: on April 30th, 2003, name is called " a kind of add the method that additive improves permanent magnetic ferrite residual magnetization " provides a kind of based on strontium or barium ferrite pre-sintered material, prepares the method for high remanent magnetism again through ultra-fine grinding, wet pressing or dry-pressing formed and high temperature sintering by secondary interpolation auxiliary agent.The additive that this invention provided is: M
xSi
yOz, any numerical value between x=1～4, y=0～2, z=2～6 wherein, M represents Fe, Pr, Nd and Sr mixture.Prepared ferrite remanent magnetism can improve 50～150Gs by 3600～4100Gs thus.The main feature of this patent of invention is: add the non rear earth oxide auxiliary agent by secondary and promote the ion substitution in strontium or the barium ferrite post forming sintering process to realize strontium or the rational space crystal structure of barium ferrite, improve ferritic remanent magnetism according to this.
Analyze more above-mentioned existing patent of invention as can be known, improve the ferrite magnetic characteristic mainly by two approach: the one, improve the ferrite magnetic characteristic by the synergy of adding pure rare earth lanthanum oxide or light lanthana and cobalt oxide; The 2nd, promote the space crystal structural transformation in strontium or the barium ferrite double sintering process to improve ferritic magnetic characteristic by adding the non rear earth oxide auxiliary agent.The common feature of two kinds of prior aries is to adopt pure compound to improve ferritic magnetic characteristic, all do not consider the synergy between the additive, in addition, because rare earth resources mostly is the mineral intergrowth material, the separation of rare earth pure compound and extraction process are very complicated, the price of corresponding pure compound is very high, then must cause the production cost of prior art for preparing rare-earth permanent magnet ferrite high thus, and the market competitiveness is fallen.
Summary of the invention
First technical problem to be solved by this invention is to be Srx (Ba) FeyOz with the molecular formula, wherein the ferrite prefiring material of the strontium of x=0.85～1, y=11～12, z=17～19 or barium is the basis, and the rare earth ore concentrate powder that is rich in lanthanum by direct interpolation prepares remanent magnetism and the better magnetic material of rare-earth permanent magnet ferrite of coercive force; Second technical problem to be solved by this invention is to be Srx (Ba) FeyOz with the molecular formula, wherein the ferrite prefiring material of the strontium of x=0.85～1, y=11～12, z=17～19 or barium is the basis, and the carbonate mixture that is rich in the rare earth ore concentrate powder of lanthanum by direct interpolation prepares remanent magnetism and the better magnetic material of rare-earth permanent magnet ferrite of coercive force.
First technical scheme of the present invention, a kind of method for preparing magnetic material of rare-earth permanent magnet ferrite comprises the following steps:
A, with the auxiliary agent that contains the ferrite prefiring material of strontium or barium and interpolation in mass ratio 85～95: 5～15 ratio joins ball mill, add entry and steel ball then and carry out the ball milling ultra-fine grinding, water is 3～1: 1 with the mass ratio of total material, steel ball is 3～8: 1 with the mass ratio of total material, obtain the hydrous slurry that particle mean size is 0.75～1.0 μ m, wherein the ferrite prefiring material of strontium or barium consists of:
Fe
2O
3 85.0～95.0％
Al
2O
3 0.1～0.6％
SrO 7.0～10.0％
BaO 0.1～0.5％
CaO 0.2～0.8％
MnO 0.2～0.5％
SiO
2 0.1～0.7％
The auxiliary agent that adds is the mixture that calcium carbonate, silicon dioxide, boric acid, cobalt oxide and the rare earth ore concentrate powder that is rich in lanthanum are formed, in the auxiliary agent of additive each component mass percent be that calcium carbonate accounts for 10.0～20.0, silica comprises 3.0～7.0, boric acid account for 3.0～7.0, cobalt oxide accounts for 0.0～20.0, all the other are the rare earth ore concentrate powder that is rich in lanthanum, the consisting of of the described rare earth ore concentrate powder that is rich in lanthanum:
La
2O
3 25.0～30.0％
CeO
2 30.0～50.0％
Nd
2O
3 6.0～16.0％
Pr
6O
11 2.0～5.0％
B, the hydrous slurry behind the above-mentioned ball milling is entered static separation moisture in the sedimentation separation drench pit, the heavy slurry time is 12～24 hours, and the ratio of height to diameter of heavy stock tank is greater than 3～1: 1, and the slip moisture content after the separation remains between 25～35%;
C, adopt wet moulding to make base substrate the slip of above-mentioned separating and dehydrating, the material feeding time of moulding process is 10～20sec, the electric current＞30A that magnetizes, and the dwell time is 10～20sec, briquetting pressure is 15～20MPa;
D, the base substrate that above-mentioned moulding is qualified are placed 24～48 hours natural air dryings in natural environment, the tunnel cave of putting into continuous propelling then carries out high temperature sintering, the sintering maximum temperature of sintering process is 1230～1320 ℃, sintering time 20～30 hours obtains described magnetic material of rare-earth permanent magnet ferrite at last.
The preferred version of such scheme is that the ferrite prefiring material of strontium or barium consists of in the steps A:
Fe
2O
3 87.0～92.0％
Al
2O
3 0.2～0.4％
SrO 8.0～9.0％
BaO 0.1～0.5％
CaO 0.2～0.5％
MnO 0.2～0.5％
SiO
2 0.2～0.5％。
The auxiliary agent mass ratio of ferrite prefiring material and interpolation is 87.5: 12.5, the auxiliary agent that adds is the mixture that calcium carbonate, silicon dioxide, boric acid, cobalt oxide and the rare earth ore concentrate powder that is rich in lanthanum are formed, in the auxiliary agent of additive each component mass percent be that calcium carbonate accounts for 15.0, silica comprises 7.0, boric acid account for 3.8, cobalt oxide accounts for 0.0～10.0, all the other are the rare earth ore concentrate powder that is rich in lanthanum, and the described rare earth ore concentrate powder that is rich in lanthanum consists of:
La
2O
3 28.0～30.0％
CeO
2 30.0～36.0％
Nd
2O
3 7.0～10.0％
Pr
6O
11 2.0～3.5％
The qualified base substrate of moulding is placed in natural environment and is not less than 26 hours and carries out drying among the step D, the tunnel cave of putting into continuous propelling then carries out high temperature sintering, the sintering maximum temperature is 1250 ℃, and sintering time 25 hours obtains described magnetic material of rare-earth permanent magnet ferrite at last.
Second technical scheme of the present invention, a kind of method for preparing magnetic material of rare-earth permanent magnet ferrite comprises the following steps:
A, with the auxiliary agent that contains the ferrite prefiring material of strontium or barium and interpolation in mass ratio 85～95: 5～15 ratio joins ball mill, add entry and steel ball then and carry out the ball milling ultra-fine grinding, water is 3～1: 1 with the mass ratio of total material, steel ball is 3～8: 1 with the mass ratio of total material, obtain the hydrous slurry that particle mean size is 0.75～1.0 μ m, wherein the ferrite prefiring material of strontium or barium is composed as follows.
The ferrite prefiring material of strontium or barium consists of:
Fe
2O
3 85.0～95.0％
Al
2O
3 0.1～0.6％
SrO 7.0～10.0％
BaO 0.1～0.5％
CaO 0.2～0.8％
MnO 0.2～0.5％
SiO
2 0.1～0.7％
The auxiliary agent that adds is the mixture that the carbonate mixture of calcium carbonate, silicon dioxide, boric acid, cobalt oxide and the rare earth ore concentrate powder that is rich in lanthanum extraction is formed, in the auxiliary agent of additive each component mass percent be that calcium carbonate accounts for 15.0～25.0, silica comprises 5.0～8.0, boric acid account for 3.0～7.0, cobalt oxide accounts for 0.0～20.0, all the other are the carbonate mixture that is rich in the rare earth ore concentrate powder extraction of lanthanum, and the carbonate mixture that the described rare earth ore concentrate powder that is rich in lanthanum extracts consists of:
La
2(CO
3)
3 17.0～24.0％
Ce(CO
3)
2 16.0～28.0％
Nd(CO
3)
2 7.0～21.0％
Pr(CO
3)
2 9.0～19.0％
B, the hydrous slurry behind the above-mentioned ball milling is entered static separation moisture in the sedimentation separation drench pit, the heavy slurry time is 12～24 hours, and the ratio of height to diameter of heavy stock tank is greater than 3～1: 1, and the slip moisture content after the separation remains between 25～35%;
C, adopt wet moulding to make base substrate the slip of above-mentioned separating and dehydrating, the material feeding time of moulding process is 10～20sec, the electric current＞30A that magnetizes, and the dwell time is 10～20sec, briquetting pressure is 15～20MPa;
D, the base substrate that above-mentioned moulding is qualified are placed 24～48 hours natural air dryings in natural environment, the tunnel cave of putting into continuous propelling then carries out high temperature sintering, the sintering maximum temperature of sintering process is 1230～1320 ℃, sintering time 20～30 hours obtains described magnetic material of rare-earth permanent magnet ferrite at last.
The preferred version of such scheme is that the ferrite prefiring material of strontium or barium consists of in the steps A:
Fe
2O
3 87.0～92.0％
Al
2O
3 0.2～0.4％
SrO 8.0～9.0％
BaO 0.1～0.5％
CaO 0.2～0.5％
MnO 0.2～0.5％
SiO
2 0.2～0.5％。
The auxiliary agent mass ratio of ferrite prefiring material and interpolation is 87.5: 12.5, the auxiliary agent that adds is the mixture that calcium carbonate, silicon dioxide, boric acid, cobalt oxide and the rare earth ore concentrate powder that is rich in lanthanum are formed, in the mixture each component mass percent be that calcium carbonate accounts for 20.0, silica comprises 7.0, boric acid account for 3.8, cobalt oxide accounts for 0.0～10.0, all the other are the carbonate mixture that is rich in the rare earth ore concentrate powder extraction of lanthanum, and the carbonate mixture that the described rare earth ore concentrate powder that is rich in lanthanum extracts consists of:
La
2(CO
3)
3 20.0～24.0％
Ce(CO
3)
2 16.0～20.0％
Nd(CO
3)
2 7.0～15.0％
Pr(CO
3)
2 9.0～12.0％
The qualified base substrate of moulding is placed in natural environment and is not less than 26 hours and carries out drying among the step D, the tunnel cave of putting into continuous propelling then carries out high temperature sintering, the sintering maximum temperature is 1250 ℃, and sintering time 25 hours obtains described magnetic material of rare-earth permanent magnet ferrite at last.
The beneficial effect of the invention is: step a of the present invention is that auxiliary agent, water, the steel ball of raw material and interpolation joins ball mill successively respectively by the processing compound requirement and carry out ultra-fine grinding with the ferrite prefiring material that contains strontium or barium, obtain the qualified hydrous slurry of particle size distribution thus, this step is rich in the rare earth ore concentrate powder of lanthanum by interpolation or is rich in the carbonate mixture that lanthanum rare earth ore concentrate powder extracts and substituted traditional pure zirconia lanthanum and cobalt oxide, simultaneously, the consumption of other auxiliary agent then also reduces accordingly, but has improved remanent magnetism, coercive force and the maximum magnetic flux energy level of permanent-magnet ferrite.The present invention has not only utilized the lanthanum element that is rich in the lanthanum lucium that strontium ion in the strontium ferrite is substituted, and utilized and be rich in the entrained cerium of lanthanum lucium and substitute cobalt oxide and improve its coercive force, also make full use of non-rare-earth substances such as being rich in the entrained iron of lanthanum lucium, silicon, calcium and aluminium, reduce the addition of corresponding these pure materials.Steps d of the present invention is one of critical process of preparation magnetic material of rare-earth permanent magnet ferrite, require the base substrate of moulding in natural environment, to place to be not less than 24 hours to carry out drying, the tunnel cave of putting into continuous propelling then carries out high temperature sintering, the sintering maximum temperature is: 1230～1320 ℃, sintering time 20～30 hours, can realize lanthanum better according to such process conditions, cerium ion forms the Magnetoplumbate-type crystal structure to the substitution effect of strontium and oxonium ion, simultaneously can guarantee the complete fusion of microcosmos area between the solid phase interface, thereby sintering goes out the product of high remanent magnetism and high-coercivity, and high density, the requirement of high strength.The rare-earth permanent magnet ferrite magnetic characteristic of the present invention's preparation can reach: Br 〉=390mT, Hcj 〉=250kA/m, BH
(MAX)〉=25kJ/m
3Therefore, the present invention not only can improve the magnetic characteristic of permanent-magnet ferrite, and can make full use of China and be rich in lanthanum rare earth resources advantage, greatly reduces the production cost of permanent-magnet ferrite.
Description of drawings
Fig. 1 is a pre-burning pellet mill back slip particle size distribution figure;
The ferrite crystal structure chart of Fig. 2 different formulations sintering;
The ferrite magnetic hysteresis line chart of Fig. 3 different formulations sintering.
Embodiment
Below by drawings and Examples the present invention is described in further detail, a kind of method for preparing the high-performance rare-earth permanent-magnetic ferrite magnetic material, it comprises the following steps:
A: contain the ferrite prefiring material of strontium or barium and the auxiliary agent of interpolation and join ball mill respectively by the requirement of quality formula rate, the auxiliary agent that wherein pre-imitation frosted glass is 85%～95%, add is 5%～15%.Add a certain proportion of water then, the mass ratio of wherein total material and water is 1: the mass ratio of (1.5～2.5) and steel ball and total material is (4～8): 1 carries out the ball milling ultra-fine grinding, obtains the hydrous slurry that particle mean size 0.75～1.0 μ m distributes thus.
B: the slurry that above-mentioned ball milling is qualified enters the static separation moisture of sedimentation separation drench pit, and the heavy slurry time is: 12～24 hours, the height of heavy stock tank and the ratio of diameter were (3～1): 1, and the slip moisture content after the separation is remained between 25～35%.
C: the slip of separating and dehydrating adopts wet moulding to be prepared into base substrate, and main molding technological condition is: material feeding time 10～20sec, the electric current＞30A that magnetizes, dwell time 10～20sec, briquetting pressure 15～20MPa.
D: the base substrate after the moulding is placed in natural environment and was carried out natural air drying in 24～48 hours, and the tunnel cave of putting into continuous propelling then carries out high temperature sintering.The sintering process condition is: the sintering maximum temperature is: 1230～1320 ℃, and sintering time: 20～30 hours.
The composition of ferrite prefiring material sees Table 1 among the step a.The auxiliary agent that adds is by calcium carbonate, silicon dioxide, boric acid, cobalt oxide and be rich in the rare earth ore concentrate powder of lanthanum or be rich in the carbonate mixture that lanthanum rare earth ore concentrate powder extracts and constitute, and wherein proportioning is: calcium carbonate 20～30%, silicon dioxide 5～10%, boric acid 2～5%, cobalt oxide 20～35%, all the other are for being rich in lanthanum material 50～70%.The composition that wherein is rich in the rare earth ore concentrate powder of lanthanum sees Table 2, be rich in the carbonate mixture that the rare earth ore concentrate powder of lanthanum extracts sees Table 3.(showing it is mass fraction in the following table)
The pre-imitation frosted glass of table 1 strontium ferrite is formed
Table 2 is rich in the composition of the rare earth ore concentrate powder of lanthanum
Table 3 is rich in the carbonate mixture of the rare earth ore concentrate powder extraction of lanthanum
Process conditions are among the step a: the auxiliary agent quality proportioning of ferrite prefiring material and interpolation is: (85～95): (5～15); The ball-milling technology condition is: water with the mass ratio of total material is: (3～1): 1.The mass ratio of total material and steel ball is 1: (3～8):.Ball milling condition is: rotating speed 3～0.5r/s, ball milling time 10～24 hours.Ball milling acceptable material particle mean size is: 5～15 μ m, particle size distribution is seen Fig. 1.The auxiliary formula that adds among the step a sees Table 4.
Table 4 secondary additive prescription
The Optimizing operation of technology of the present invention requires:
Ingredient requirement among the step a is: the ferrite prefiring material composition of strontium or barium sees Table 5, and the rare earth ore concentrate powder composition that is rich in lanthanum sees Table 6, and the carbonate mixture composition that is rich in the extraction of lanthanum rare earth ore concentrate powder sees Table 7.
The pre-imitation frosted glass of table 5 strontium ferrite is formed
Table 6 is rich in the composition of the rare earth ore concentrate powder of lanthanum
Table 7 is rich in the carbonate mixture of the rare earth ore concentrate powder extraction of lanthanum
The auxiliary agent that adds among the step a is by calcium carbonate, silicon dioxide, boric acid, cobalt oxide and be rich in the rare earth ore concentrate powder of lanthanum or be rich in the carbonate mixture that lanthanum rare earth ore concentrate powder extracts and constitute, and the purity of calcium carbonate, silicon dioxide, boric acid, cobalt oxide is greater than 98%, and its prescription composition sees Table 8.The auxiliary agent quality proportioning of ferrite prefiring material and interpolation is: 87.5: 12.5.
Table 8 secondary additive prescription
The qualified base substrate of moulding is placed in natural environment and is not less than 26 hours and carries out drying in the steps d, and the tunnel cave of putting into continuous propelling then carries out high temperature sintering, and the sintering maximum temperature is: 1250 ℃, and sintering time: 25 hours.
Ferrite prefiring material sees Table 9 with the batching of secondary interpolation auxiliary agent among the different embodiment, and the magnetic sample characteristic sees Table 10 behind the sintering, and corresponding crystal structure sees that Fig. 2, magnetic hysteresis loop see Fig. 3.
Table 9 rare-earth permanent magnet ferrite composition of raw materials
Described content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (4)
1. a method for preparing magnetic material of rare-earth permanent magnet ferrite comprises the following steps:
A, with the auxiliary agent that contains the ferrite prefiring material of strontium or barium and interpolation in mass ratio 85～95: 5～15 ratio joins ball mill, add entry and steel ball then and carry out the ball milling ultra-fine grinding, water is 3～1: 1 with the mass ratio of total material, steel ball is 3～8: 1 with the mass ratio of total material, obtain the hydrous slurry that particle mean size is 0.75～1.0 μ m, wherein the ferrite prefiring material of strontium or barium consists of:
Fe
2O
3 85.0～95.0％
Al
2O
3 0.1～0.6％
SrO 7.0～10.0％
BaO 0.1～0.5％
CaO 0.2～0.8％
MnO 0.2～0.5％
SiO
2 0.1～0.7％
The auxiliary agent that adds is the mixture that calcium carbonate, silicon dioxide, boric acid, cobalt oxide and the rare earth ore concentrate powder that is rich in lanthanum are formed, in the auxiliary agent of additive each component mass percent be that calcium carbonate accounts for 10.0～20.0, silica comprises 3.0～7.0, boric acid account for 3.0～7.0, cobalt oxide accounts for 0.0～20.0, all the other are the rare earth ore concentrate powder that is rich in lanthanum, the consisting of of the described rare earth ore concentrate powder that is rich in lanthanum:
La
2O
3 25.0～30.0％
CeO
2 30.0～50.0％
Nd
2O
3 6.0～16.0％
Pr
6O
11 2.0～5.0％
B, the hydrous slurry behind the above-mentioned ball milling is entered static separation moisture in the sedimentation separation drench pit, the heavy slurry time is 12～24 hours, and the ratio of height to diameter of heavy stock tank is greater than 3～1: 1, and the slip moisture content after the separation remains between 25～35%;
C, adopt wet moulding to make base substrate the slip of above-mentioned separating and dehydrating, the material feeding time of moulding process is 10～20sec, the electric current＞30A that magnetizes, and the dwell time is 10～20sec, briquetting pressure is 15～20MPa;
D, the base substrate that above-mentioned moulding is qualified are placed 24～48 hours natural air dryings in natural environment, the tunnel cave of putting into continuous propelling then carries out high temperature sintering, the sintering maximum temperature of sintering process is 1230～1320 ℃, sintering time 20～30 hours obtains described magnetic material of rare-earth permanent magnet ferrite at last.
2. according to the described method for preparing magnetic material of rare-earth permanent magnet ferrite of claim 1, it is characterized in that the ferrite prefiring material of strontium in the steps A or barium consists of:
Fe
2O
3 87.0～92.0％
A1
2O
3 0.2～0.4％
SrO 8.0～9.0％
BaO 0.1～0.5％
CaO 0.2～0.5％
MnO 0.2～0.5％
SiO
2 0.2～0.5％。
The auxiliary agent mass ratio of ferrite prefiring material and interpolation is 87.5: 12.5, the auxiliary agent that adds is the mixture that calcium carbonate, silicon dioxide, boric acid, cobalt oxide and the rare earth ore concentrate powder that is rich in lanthanum are formed, in the auxiliary agent of additive each component mass percent be that calcium carbonate accounts for 15.0, silica comprises 7.0, boric acid account for 3.8, cobalt oxide accounts for 0.0～10.0, all the other are the rare earth ore concentrate powder that is rich in lanthanum, and the described rare earth ore concentrate powder that is rich in lanthanum consists of:
La
2O
3 28.0～30.0％
CeO
2 30.0～36.0％
Nd
2O
3 7.0～10.0％
Pr
6O
11 2.0～3.5％
The qualified base substrate of moulding is placed in natural environment and is not less than 26 hours and carries out drying among the step D, the tunnel cave of putting into continuous propelling then carries out high temperature sintering, the sintering maximum temperature is 1250 ℃, and sintering time 25 hours obtains described magnetic material of rare-earth permanent magnet ferrite at last.
3. a method for preparing magnetic material of rare-earth permanent magnet ferrite comprises the following steps:
A, with the auxiliary agent that contains the ferrite prefiring material of strontium or barium and interpolation in mass ratio 85～95: 5～15 ratio joins ball mill, add entry and steel ball then and carry out the ball milling ultra-fine grinding, water is 3～1: 1 with the mass ratio of total material, steel ball is 3～8: 1 with the mass ratio of total material, obtain the hydrous slurry that particle mean size is 0.75～1.0 μ m, wherein the ferrite prefiring material of strontium or barium is composed as follows.
The ferrite prefiring material of strontium or barium consists of:
Fe
2O
3 85.0～95.0％
Al
2O
3 0.1～0.6％
SrO 7.0～10.0％
BaO 0.1～0.5％
CaO 0.2～0.8％
MnO 0.2～0.5％
SiO
2 0.1～0.7％
The auxiliary agent that adds is the mixture that the carbonate mixture of calcium carbonate, silicon dioxide, boric acid, cobalt oxide and the rare earth ore concentrate powder that is rich in lanthanum extraction is formed, in the auxiliary agent of additive each component mass percent be that calcium carbonate accounts for 15.0～25.0, silica comprises 5.0～8.0, boric acid account for 3.0～7.0, cobalt oxide accounts for 0.0～20.0, all the other are the carbonate mixture that is rich in the rare earth ore concentrate powder extraction of lanthanum, and the carbonate mixture that the described rare earth ore concentrate powder that is rich in lanthanum extracts consists of:
La
2(CO
3)
3 17.0～24.0％
Ce(CO
3)
2 16.0～28.0％
Nd(CO
3)
2 7.0～21.0％
Pr(CO
3)
2 9.0～19.0％
B, the hydrous slurry behind the above-mentioned ball milling is entered static separation moisture in the sedimentation separation drench pit, the heavy slurry time is 12～24 hours, and the ratio of height to diameter of heavy stock tank is greater than 3～1: 1, and the slip moisture content after the separation remains between 25～35%;
C, adopt wet moulding to make base substrate the slip of above-mentioned separating and dehydrating, the material feeding time of moulding process is 10～20sec, the electric current＞30A that magnetizes, and the dwell time is 10～20sec, briquetting pressure is 15～20MPa;
D, the base substrate that above-mentioned moulding is qualified are placed 24～48 hours natural air dryings in natural environment, the tunnel cave of putting into continuous propelling then carries out high temperature sintering, the sintering maximum temperature of sintering process is 1230～1320 ℃, sintering time 20～30 hours obtains described magnetic material of rare-earth permanent magnet ferrite at last.
4. according to the described method for preparing magnetic material of rare-earth permanent magnet ferrite of claim 3, it is characterized in that the ferrite prefiring material of strontium in the steps A or barium consists of:
Fe
2O
3 87.0～92.0％
Al
2O
3 0.2～0.4％
SrO 8.0～9.0％
BaO 0.1～0.5％
CaO 0.2～0.5％
MnO 0.2～0.5％
SiO
2 0.2～0.5％。
The auxiliary agent mass ratio of ferrite prefiring material and interpolation is 87.5: 12.5, the auxiliary agent that adds is the mixture that calcium carbonate, silicon dioxide, boric acid, cobalt oxide and the rare earth ore concentrate powder that is rich in lanthanum are formed, in the mixture each component mass percent be that calcium carbonate accounts for 20.0, silica comprises 7.0, boric acid account for 3.8, cobalt oxide accounts for 0.0～10.0, all the other are the carbonate mixture that is rich in the rare earth ore concentrate powder extraction of lanthanum, and the carbonate mixture that the described rare earth ore concentrate powder that is rich in lanthanum extracts consists of:
La
2(CO
3)
3 20.0～24.0％
Ce(CO
3)
2 16.0～20.0％
Nd(CO
3)
2 7.0～15.0％
Pr(CO
3)
2 9.0～12.0％
The qualified base substrate of moulding is placed in natural environment and is not less than 26 hours and carries out drying among the step D, the tunnel cave of putting into continuous propelling then carries out high temperature sintering, the sintering maximum temperature is 1250 ℃, and sintering time 25 hours obtains described magnetic material of rare-earth permanent magnet ferrite at last.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870579A (en) * | 2010-06-10 | 2010-10-27 | 上海应用技术学院 | Permanently magnetic strontium ferrite material and preparation method thereof |
| CN101786869B (en) * | 2009-12-30 | 2012-06-13 | 安徽大学 | Calcium permanent magnetic ferrite material and preparation method thereof |
| CN102731080A (en) * | 2012-07-13 | 2012-10-17 | 当涂县海川磁性材料有限公司 | Processing method for preparing powder used for ferrite magnetic material |
| CN103833343A (en) * | 2014-03-01 | 2014-06-04 | 南通飞来福磁铁有限公司 | Nano rare-earth permanent magnet material |
| CN110467452A (en) * | 2019-09-25 | 2019-11-19 | 横店集团东磁股份有限公司 | A kind of permanent-magnet material and preparation method thereof |
| CN113698191A (en) * | 2020-05-22 | 2021-11-26 | 盐城市中天磁材有限公司 | Rare earth-substituted strontium ferrite and preparation method thereof |
| CN113896522A (en) * | 2021-11-12 | 2022-01-07 | 深圳信义磁性材料有限公司 | Permanent magnetic ferrite and preparation method thereof |
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| CN101786869B (en) * | 2009-12-30 | 2012-06-13 | 安徽大学 | Calcium permanent magnetic ferrite material and preparation method thereof |
| CN101870579A (en) * | 2010-06-10 | 2010-10-27 | 上海应用技术学院 | Permanently magnetic strontium ferrite material and preparation method thereof |
| CN102731080A (en) * | 2012-07-13 | 2012-10-17 | 当涂县海川磁性材料有限公司 | Processing method for preparing powder used for ferrite magnetic material |
| CN103833343A (en) * | 2014-03-01 | 2014-06-04 | 南通飞来福磁铁有限公司 | Nano rare-earth permanent magnet material |
| CN103833343B (en) * | 2014-03-01 | 2015-08-26 | 南通飞来福磁铁有限公司 | A kind of nano rare earth permanent-magnet ferrite material |
| CN110467452A (en) * | 2019-09-25 | 2019-11-19 | 横店集团东磁股份有限公司 | A kind of permanent-magnet material and preparation method thereof |
| CN113698191A (en) * | 2020-05-22 | 2021-11-26 | 盐城市中天磁材有限公司 | Rare earth-substituted strontium ferrite and preparation method thereof |
| CN113896522A (en) * | 2021-11-12 | 2022-01-07 | 深圳信义磁性材料有限公司 | Permanent magnetic ferrite and preparation method thereof |
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