CN102898127B - Sintered permanent magnetic ferrite and manufacture method thereof - Google Patents
Sintered permanent magnetic ferrite and manufacture method thereof Download PDFInfo
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Abstract
The invention provides a sintered permanent magnetic ferrite and a manufacture method thereof. The manufacture method for the sintered permanent magnetic ferrite comprises the following steps of: mixing weighed raw materials according to a composition formula of (1-x)AO(x/2)R2O3(n-z-y/2)Fe2O3zM2O3yTiO2 to obtain mixture of which the average granularity is less than 1.0 micrometer; at the temperature of 1160-1260DEG C, sintering the mixture for the first time to obtain the powder of the mixture; in the preset percentage by mass, adding dispersing agent into the powder of the mixture; grinding to obtain slurry of which the average granularity is 0.7-0.9 micrometer; regulating the water content of the slurry to occupy 30-45wt% of the slurry; forming the slurry in a magnetic field to obtain a forming body; carrying out thermal treatment to the forming body at the temperature of 100-500DEG C; carrying out secondary sintering at the temperature of 1180-1220DEG C; and obtaining the sintered permanent magnetic ferrite after the temperature is kept for the preset time. The invention provides the sintered permanent magnetic ferrite and the manufacture method thereof, wherein the sintered permanent magnetic ferrite has a high forming efficiency when being formed in the magnetic field and has an excellent magnetic performance, and a product is unlikely to crack when being sintered.
Description
Technical field
The present invention relates to a kind of sintered permanent ferrite and manufacture method thereof, belong to the magnetic composite technical field.
Background technology
Sintered permanent ferrite is owing to having higher magnetic property, erosion resistance and cheaper price, therefore be widely used in automobile and household electric appliances.Sintered permanent ferrite adopts strontium ferrites or the barium ferrite of Magnetoplumbate-type (M type) to fire magnet more at present.The parameter that characterizes the magnet magnetic property mainly contains two, i.e. residual flux density (Br) and HCJ (Hcj).
The Br of magnet is the density that is proportional to magnet, the orientation degree of magnet and the saturation magnetization determined by crystalline structure.Take strontium ferrites as example, and the theoretical value of its saturation magnetization is about 465mT, but, due to the restriction of density and orientation degree, makes the Br of traditional strontium ferrites be at most 446mT, realizes that in prior art Br is greater than 450mT basically impossible.
The Hcj of magnet is directly proportional to the product (HA * fc) that anisotropy field (HA=2K1/Is) is multiplied by single domain crystal grain mark (fc).K1 is the magnetocrystalline anisotropy constant determined by crystalline structure.K1=3.3 * 106erg/cm3 that M type barium ferrite has, K1=3.5 * 106erg/cm3 that M type strontium ferrites has.In conventional art, M type strontium ferrites has maximum K1, is difficult to realize the further improvement of K1.Therefore will improve the Hcj of magnet, will make the single domain crystal grain in magnet many as much as possible, this is because ferrite crystal grains while being single domain, can realize in maximum grasping coercivity H j.
Take strontium ferrites as example, and its single-domain critical size is about 1 μ m, therefore wants to obtain larger coercive force, just the grain-size of sintered magnet must be controlled in 1 μ m.Consider the growth of sintering crystal grain in the stage, the particle size in compression molding stage should be controlled in 0.5 μ m.But the particle of this size easily causes the reduction of production efficiency, and magnet easily ftractures.
In existing magnet manufacturing process, in order to obtain excellent magnetic property, require moulding to use the average particle size of slip lower than 0.7 micron, this just causes slip in moulding process, water discharge time extends, and shaping efficiency declines to a great extent, thereby causes the manufacturing cost of ferrite sintered body magnet to increase.As mean particle size is greater than 0.7 micron, shaping efficiency will obviously improve, but magnetic property can reduce along with the increase of mean particle size.
Summary of the invention
The problem that shaping efficiency lower, magnetic property lower of the present invention for existing in the existing magnet manufacturing technology of solution, and then a kind of sintered permanent ferrite and manufacture method thereof are provided.For this reason, the invention provides following technical scheme:
A kind of sintered permanent ferrite, described sintered permanent ferrite be take hexagonal ferrite as principal phase, and containing element A, R, M, Ti and Fe, and has the molecular formula of following characteristics:
(1－x)AO(x/2)R
2O
3(n-z-y/2)Fe
2O
3zM
2O
3yTiO
2；
Corresponding elements A means at least one element in Sr or Ba; Element R is illustrated at least one element be selected from rare earth element and Y, and necessary containing element La; Element M means at least one element in Co, Mn or Zn, and necessary containing element Co; X, y, z means respectively the mole number of each metal oxide, and n means mol ratio, wherein, and 0.04≤x≤0.5,0.04≤z≤0.4,0.005≤y≤0.15,5.5≤n≤6.0.
A kind of manufacture method of sintered permanent ferrite comprises:
According to composition formula (1-x) AO (x/2) R
2o
3(n-z-y/2) Fe
2o
3zM
2o
3yTiO
2the starting material that take are obtained to the mixture that mean particle size is less than 1.0 microns by mixing;
Described mixture is carried out once sinteredly under the condition of 1160 ℃～1260 ℃, obtain the powder of described mixture;
Add dispersion agent by predetermined mass percent in the powder of described mixture, and obtain by grinding the slip that mean particle size is 0.7～0.9 micron;
The mass percent that the water content of described slip is adjusted in described slip is 30%～45%, and, by the moulding in magnetic field of described slip, obtains formed body;
Described formed body is heat-treated under the condition of 100 ℃～500 ℃, and carry out double sintering under the condition of 1180 ℃～1220 ℃, obtain described sintered permanent ferrite after the insulation scheduled time.
The invention provides a kind of in magnetic field during moulding shaping efficiency high, when sintering, product is not easy cracking, the ferrite sintered body of magnetic property excellence and manufacture method thereof.
The accompanying drawing explanation
The technical scheme that Fig. 1 provides by embodiment 4 for the present invention obtains the magnetic property schematic diagram of sintered compact.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making all other embodiment that obtain under the creative work prerequisite, belong to the scope of protection of the invention.
The specific embodiment of the present invention provides a kind of sintered permanent ferrite, and described sintered permanent ferrite be take hexagonal ferrite as principal phase, and containing element A, R, M, Ti and Fe, and has the molecular formula of following characteristics:
(1－x)AO(x/2)R
2O
3(n-z-y/2)Fe
2O
3?zM
2O
3?yTiO
2；
Corresponding elements A means at least one element in Sr or Ba; Element R is illustrated at least one element be selected from rare earth element and Y, and necessary containing element La; Element M means at least one element in Co, Mn or Zn, and necessary containing element Co; X, y, z means respectively the mole number of each metal oxide, and n means mol ratio, wherein, and 0.04≤x≤0.5,0.04≤z≤0.4,0.005≤y≤0.15,5.5≤n≤6.0.
By add appropriate Ti in sintered permanent ferrite
4+, make during element ti can enter ferrite lattice in the pre-burning process, thereby improve the microscopic appearance of ferrite sintered body powder and magnet, and can effectively suppress the growth of crystal grain, reduce pore, thereby significantly improved the magnetic property of material.
The specific embodiment of the present invention also provides a kind of manufacture method of sintered permanent ferrite, comprising:
According to composition formula (1-x) AO (x/2) R
2o
3(n-z-y/2) Fe
2o
3zM
2o
3yTiO
2the starting material that take are obtained to the mixture that mean particle size is less than 1.0 microns by mixing;
Described mixture is carried out once sinteredly under the condition of 1160 ℃～1260 ℃, obtain the powder of described mixture;
Add dispersion agent by predetermined mass percent in the powder of described mixture, and obtain by grinding the slip that mean particle size is 0.7～0.9 micron;
The mass percent that the water content of described slip is adjusted in described slip is 30%～45%, and, by the moulding in magnetic field of described slip, obtains formed body;
Described formed body is heat-treated under the condition of 100 ℃～500 ℃, and carry out double sintering under the condition of 1180 ℃～1220 ℃, obtain described sintered permanent ferrite after the insulation scheduled time.
Preferably, corresponding dispersion agent can be for accounting for the polycarboxylate that described raw-material mass percent is 0.4～1.5%.Although adopt traditional dispersion agent (as calglucon) also can improve a certain amount of magnet performance, but adopt polycarboxylate to add after once sintered as dispersion agent, not only can improve orientation degree, can also crystal grain thinning, improve coercive force, compare the further magnetic property that improved with traditional dispersion agent.
Technical scheme the present invention proposed below by specific embodiment elaborates.
Embodiment 1
Adopt following starting material:
Fe
2o
3powder (purity>=99.3%, contain the impurity such as Mn, mean particle size≤0.7 μ m), addition is 84.5wt%;
SrCO
3powder (purity>=98.0% contains the impurity such as Ba, Ca, mean particle size≤2 μ m), addition is 10.9wt%;
La
2o
3powder (purity>=99.9%, mean particle size≤2 μ m), addition is 3.0wt%;
Co
2o
3powder (purity>=99.0%, mean particle size≤2 μ m), addition is 1.5wt%;
TiO
2powder (purity>=99.0%, mean particle size≤1 μ m), addition is 0.1wt%;
Above-mentioned mass percent is taken to each component starting material, and add several additive, adopt the dry method mode to mix, carry out subsequently granulation, and carry out once sinteredly in air in 1200 ℃, be incubated 2 hours, obtain Preburning material, its grain-size is controlled at 1～2 μ m, and grain size is even, and pore is few.The principal phase that this Preburning material ferrite has is:
0.8SrO?0.1La
2O
3?5.765Fe
2O
3?0.1Co
2O
3?0.01TiO
2
The gained Preburning material is carried out in the dry type vibratory ball mill to the coarse reduction of 20 minutes, the material powder mean particle size after pulverizing is 3.0 μ m, takes above-mentioned powder 300g, adds the CaCO of 1.4wt%
3, the SiO of 0.6wt%
2, do not add dispersion agent, the 500ml deionized water, in wet ball-milling, continuously grinding is 12 hours, and the mean particle size of the slip particle after pulverizing is 0.8 μ m.
The water content of slip is adjusted to 40wt%, then compression moulding in magnetic field, magneticstrength is 8000Oe, and pressure is 5MPa, and the gained pressed compact is diameter 35.2mm, the right cylinder of height 15mm.
At 100～500 ℃, pressed compact is heat-treated, organic dispersing agent is divided and takes off, sintering in air then, temperature rise rate is 100 ℃/hs, then 1210 insulation 2 hours, obtains sintered compact, after its upper and lower surface grind to processing, the measurement magnetic property.
The comparative example 1, if do not add TiO in starting material
2, the grain-size that obtains Preburning material can only reach at 2～4 μ m, and grain size differs, and pore is many.The principal phase that this Preburning material ferrite has is:
0.8SrO?0.1La
2O
3?5.77Fe
2O
3?0.1Co
2O
3
All the other are identical with embodiment 1.Embodiment 1 is as shown in the table with comparative example 1 comparison of magnetic property:
Embodiment 2
The Preburning material that adopts embodiment 1 to obtain, the CaCO of interpolation 1.4wt% before Preburning material is pulverized
3, the SiO of 0.6wt%
2, the polycarboxylate of 1.5wt%, the 500ml deionized water, rest part is identical with embodiment 1, measures magnetic property.
The comparative example 2
The Preburning material that adopts embodiment 1 to obtain, the CaCO of interpolation 1.4wt% before Preburning material is pulverized
3, the SiO of 0.6wt%
2, the calglucon of 1.5wt% is as dispersion agent, the 500ml deionized water, and rest part is identical with embodiment 1, measures magnetic property.
Embodiment 2 is as shown in the table with comparative example 2 comparison of magnetic property:
Embodiment 3
The Preburning material that adopts embodiment 1 to obtain carries out the gained Preburning material coarse reduction of 20 minutes in the dry type vibratory ball mill, and the material powder mean particle size after pulverizing is 3.0 μ m, takes above-mentioned powder 300g, adds the CaCO of 1.4wt%
3, the SiO of 0.6wt%
2, the polycarboxylate of 1.5wt%, the 500ml deionized water, continuously grinding in wet ball-milling, by adjusting Ball-milling Time, the mean particle size that obtains the slip particle is 0.9 μ m, 0.85 μ m, 0.8 μ m, 0.75 μ m, 0.69 μ m, 0.65 μ m, 0.59 μ m.
The water content of slip is adjusted to 40wt%, then compression moulding in magnetic field, magneticstrength is 8000Oe, and pressure is 5MPa, and the gained pressed compact is diameter 35.2mm, the right cylinder of height 15mm.
At 100～500 ℃, pressed compact is heat-treated, organic dispersing agent is divided and takes off, sintering in air then, temperature rise rate is 100 ℃/hs, then 1210 insulation 2 hours, obtains sintered compact, after its upper and lower surface grind to processing, the measurement magnetic property.
The comparative example 3, adopt following starting material:
Fe
2o
3powder (purity>=99.3%, contain the impurity such as Mn, mean particle size≤0.7 μ m), addition is 83.8wt%;
SrCO
3powder (purity>=98.0% contains the impurity such as Ba, Ca, mean particle size≤1.3 μ m), addition is 9.5wt%;
La
2o
3powder (purity>=99.9% contains the impurity such as Ba, Ca, mean particle size≤0.7 μ m), addition is 4.5wt%
Co
3o
4powder (purity>=99.0% contains the impurity such as Ba, Ca, mean particle size≤0.7 μ m), addition is 2.2wt%
Above-mentioned mass percent is taken to each component starting material, and add several additive, adopt the dry method mode to mix, carry out subsequently granulation, and carry out once sinteredly in air in 1200 ℃, be incubated 2 hours, obtain Preburning material, the principal phase that makes this Preburning material ferrite have is:
0.7SrO?0.15La
2O
3?5.73Fe
2O
3?0.15Co
2O
3
The gained Preburning material is carried out in the dry type vibratory ball mill to the coarse reduction of 20 minutes, the material powder mean particle size after pulverizing is 3.0 μ m, takes above-mentioned powder 300g, adds the CaCO of 1.4wt%
3, the SiO of 0.6wt%
2, the calglucon of 1.5wt%, the 500ml deionized water, continuously grinding in wet ball-milling, by adjusting Ball-milling Time, the mean particle size that obtains the slip particle is 0.80 μ m, 0.69 μ m, 0.59 μ m.
The water content of slip is adjusted to 40wt%, then compression moulding in magnetic field, magneticstrength is 8000Oe, and pressure is 5MPa, and the gained pressed compact is diameter 35.2mm, the right cylinder of height 15mm.
At 100～500 ℃, pressed compact is heat-treated, organic dispersing agent is divided and takes off, sintering in air then, temperature rise rate is 100 ℃/hs, then 1210 insulation 2 hours, obtains sintered compact, after its upper and lower surface grind to processing, the measurement magnetic property.
Embodiment 3 is as shown in the table with comparative example 3 comparison of magnetic property:
Embodiment 4, adopt following starting material:
Fe
2o
3powder (purity>=99.3%, contain the impurity such as Mn, mean particle size≤0.7 μ m), addition is 84.5wt%;
SrCO
3powder (purity>=98.0% contains the impurity such as Ba, Ca, mean particle size≤2 μ m), addition is 10.9wt%;
La
2o
3powder (purity>=99.9%, mean particle size≤2 μ m), addition is 3.0wt%;
Co
3o
4powder (purity>=99.0%, mean particle size≤2 μ m), addition is 1.5wt%;
TiO
2powder (purity>=99.0%, mean particle size≤1 μ m), addition is 0.05～0.2wt%.
Above-mentioned mass percent is taken to each component starting material, and add several additive, adopt the dry method mode to mix, carry out subsequently granulation, and carry out once sinteredly in air in 1200 ℃, be incubated 2 hours, obtain Preburning material, the principal phase that makes this Preburning material ferrite have is:
0.8SrO?0.1La
2O
3?5.765Fe
2O
3?0.1Co
2O
3(0.005～0.02)TiO
2
The gained Preburning material is carried out in the dry type vibratory ball mill to the coarse reduction of 20 minutes, the material powder mean particle size after pulverizing is 3.0 μ m, takes above-mentioned powder 300g, adds the CaCO of 1.4wt%
3, the SiO of 0.6wt%
2, the polycarboxylate of 1.5wt%, the 500ml deionized water, in wet ball-milling, continuously grinding 12, and the mean particle size that obtains the slip particle is 0.8 μ m.
The water content of slip is adjusted to 40wt%, then compression moulding in magnetic field, magneticstrength is 8000Oe, and pressure is 5MPa, and the gained pressed compact is diameter 35.2mm, the right cylinder of height 15mm.
At 100～500 ℃, pressed compact is heat-treated, organic dispersing agent is divided and takes off, sintering in air then, temperature rise rate is 100 ℃/hs, then 1210 insulation 2 hours, obtains sintered compact, after its upper and lower surface grind to processing, the measurement magnetic property.As shown in Figure 1.
The technical scheme that adopts this embodiment to provide, a small amount of Ti
4+add, can significantly improve the microscopic appearance of M type ferrite sintered body, suppress the misgrowth of crystal grain, reduce pore, thereby obviously improve the characteristic of ferrite sintered body powder, and significantly improve magnet performance; Make dispersion agent at special 0.4～1.5wt% polycarboxylate that adds of broken stage of fine powder, make when sintering, can effectively control the growth of crystal grain, crystal grain thinning, thus effectively improve coercive force; Optimization design, particularly y=0.01(by formula are Ti=0.1wt%) time, adopting mean particle size is 0.8 μ m, be easy to draining, the slip that shaping efficiency is high, can obtain Br=451mT, the ferrite sintered body material of the magnet performance excellence of Hcj=382kA/m.
The above; it is only preferably embodiment of the present invention; but protection scope of the present invention is not limited to this; anyly be familiar with those skilled in the art in the technical scope that the embodiment of the present invention discloses; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (5)
1. the manufacture method of a sintered permanent ferrite, described sintered permanent ferrite be take hexagonal ferrite as principal phase, and containing element A, R, M, Ti and Fe, and has the molecular formula of following characteristics:
(1－x)AO(x/2)R
2O
3(n-z-y/2)Fe
2O
3zM
2O
3yTiO
2；
Corresponding elements A means at least one element in Sr or Ba; Element R is illustrated at least one element be selected from rare earth element and Y, and necessary containing element La; Element M means at least one element in Co, Mn or Zn, and necessary containing element Co; X, y, z means respectively the mole number of each metal oxide, and n means mol ratio, wherein, and 0.04≤x≤0.5,0.04≤z≤0.4,0.005≤y≤0.15,5.5≤n≤6.0.
It is characterized in that, the manufacture method of described sintered permanent ferrite comprises:
According to composition formula (1-x) AO (x/2) R
2o
3(n-z-y/2) Fe
2o
3zM
2o
3yTiO
2the starting material that take are obtained to the mixture that mean particle size is less than 1.0 microns by mixing, and described starting material comprise Fe
2o
3, SrCO
3, La
2o
3, Co
2o
3and TiO
2, described Fe
2o
3mass percent in described starting material is 84.5%, described SrCO
3mass percent in described starting material is 10.9%, described La
2o
3mass percent in described starting material is 3.0%, described Co
2o
3mass percent in described starting material is 1.5%, described TiO
2mass percent in described starting material is 0.1%;
Described mixture is carried out once sinteredly under the condition of 1160 ℃～1260 ℃, obtain the powder of described mixture;
Add dispersion agent by predetermined mass percent in the powder of described mixture, and obtain by grinding the slip that mean particle size is 0.7～0.9 micron;
The mass percent that the water content of described slip is adjusted in described slip is 30%～45%, and, by the moulding in magnetic field of described slip, obtains formed body;
Described formed body is heat-treated under the condition of 100 ℃～500 ℃, and carry out double sintering under the condition of 1180 ℃～1220 ℃, obtain described sintered permanent ferrite after the insulation scheduled time.
2. manufacture method according to claim 1, is characterized in that, described dispersion agent is to account for the polycarboxylate that described raw-material mass percent is 0.4～1.5%.
3. manufacture method according to claim 1, is characterized in that, the CaCO that the mass percent that adds the powder that accounts for described mixture in the powder of described mixture is 1.4%
3, 0.6% SiO
2with 1.5% polycarboxylate.
4. the manufacture method of a sintered permanent ferrite, described sintered permanent ferrite be take hexagonal ferrite as principal phase, and containing element A, R, M, Ti and Fe, and has the molecular formula of following characteristics:
(1－x)AO(x/2)R
2O
3(n-z-y/2)Fe
2O
3zM
2O
3yTiO
2；
Corresponding elements A means at least one element in Sr or Ba; Element R is illustrated at least one element be selected from rare earth element and Y, and necessary containing element La; Element M means at least one element in Co, Mn or Zn, and necessary containing element Co; X, y, z means respectively the mole number of each metal oxide, and n means mol ratio, wherein, and 0.04≤x≤0.5,0.04≤z≤0.4,0.005≤y≤0.15,5.5≤n≤6.0.
It is characterized in that, the manufacture method of described sintered permanent ferrite comprises:
According to composition formula (1-x) AO (x/2) R
2o
3(n-z-y/2) Fe
2o
3zM
2o
3yTiO
2the starting material that take are obtained to the mixture that mean particle size is less than 1.0 microns by mixing, and described starting material comprise Fe
2o
3, SrCO
3, La
2o
3, Co
3o
4and TiO
2, described Fe
2o
3mass percent in described starting material is 84.5%, described SrCO
3mass percent in described starting material is 10.9%, described La
2o
3mass percent in described starting material is 3.0%, described Co
3o
4mass percent in described starting material is 1.5%, described TiO
2mass percent in described starting material is 0.05～0.2%;
Described mixture is carried out once sinteredly under the condition of 1160 ℃～1260 ℃, obtain the powder of described mixture;
Add dispersion agent by predetermined mass percent in the powder of described mixture, and obtain by grinding the slip that mean particle size is 0.7～0.9 micron;
The mass percent that the water content of described slip is adjusted in described slip is 30%～45%, and, by the moulding in magnetic field of described slip, obtains formed body;
Described formed body is heat-treated under the condition of 100 ℃～500 ℃, and carry out double sintering under the condition of 1180 ℃～1220 ℃, obtain described sintered permanent ferrite after the insulation scheduled time.
5. manufacture method according to claim 4, is characterized in that, the CaCO that the mass percent that adds the powder that accounts for described mixture in the powder of described mixture is 1.4%
3, 0.6% SiO
2with 1.5% polycarboxylate.
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