CN100368344C - Preparation process of anisotropic permanent magnetic ferrite - Google Patents
Preparation process of anisotropic permanent magnetic ferrite Download PDFInfo
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- CN100368344C CN100368344C CNB2006100356986A CN200610035698A CN100368344C CN 100368344 C CN100368344 C CN 100368344C CN B2006100356986 A CNB2006100356986 A CN B2006100356986A CN 200610035698 A CN200610035698 A CN 200610035698A CN 100368344 C CN100368344 C CN 100368344C
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Abstract
The present invention discloses a preparation method of an anisotropic permanent magnetic ferrite, which comprises: mixing ferrite powder with a polymer adhesive to prepare powder; pressing for forming; sintering. The polymer adhesive contains 60% to 75% (by mass) of copolymer of polyamide, polyethylene and fluorine-containing polyethylene and 25% to 40% (by mass) of zinc stearate. The adopted polymer adhesive has the advantages of good adhesive property, lubricating property, environmental friendliness, no harm and small environment pollution to human bodies during production. The magnetic property of the prepared anisotropic permanent magnetic ferrite is high and is close to the level of magnetic powder of the same grade by a wet method; residual magnetism reaches 96.9% of the products prepared by the wet method, maximum magnetic energy product can reach 93.8% of the products prepared by the wet method, and induction coercive force and intrinsic coercive force can reach more than 100% of those of the products prepared by the wet method. The production cost of all products of the anisotropic permanent magnetic ferrite which are produced by a dry method can be greatly reduced by using the preparation method.
Description
Technical field
The present invention relates to method for preparing permanent magnetic ferrite, particularly a kind of anisotropy method for preparing permanent magnetic ferrite.
Background technology
Traditional forming method of anisotropy permanent-magnet ferrite has two kinds of wet moulding and dry-press processes.Traditional wet moulding is binding agent and lubricant with water, and its product performance are high and stable; But because wet moulding must be removed the most of moisture in the mould in pressure process, and the blank of compression moulding must just can enter sintering circuit after the drying, exists therefore that molding time is long, production efficiency is low, yield rate is low, the mould structure complexity of shaped device, is difficult to the shortcoming that realizes that automation size is produced.Traditional dry-press process is used solid-state binding agent, as calcium stearate, barium stearate, naphthalene, polyvinyl alcohol, camphor etc.; Calcium stearate is non-volatile at normal temperatures, odorlessness, oilness are fine, but the magnetic property that cohesiveness is not good, the residuals that produces after the blank bad mechanical strength of compression moulding, sintering can reduce product; Barium stearate is similar to calcium stearate, but oilness is slightly poor; Naphthalene has flake-like crystal, is difficult to the magnetic highly dispersed and uniform mixing, and pore is more in the magnet, and orientation degree is not good; Cohesiveness was very strong but oilness is very poor when polyvinyl alcohol was moist, and it is agglomerating that magnetic is assembled, no adhesion; Camphor has good lubricity and cohesiveness, is the most frequently used binding agent, but the volatility of camphor and pungency are all very strong and harmful, and heavy dose of contact can cause the cardiomotility paralysis so that cause serious spasm.In addition, adopt the magnetic of same levels, the product magnetic property of dry-press process is relatively poor, generally has only 80～90% of wet moulding product.If will improve the product magnetic property of dry-press process, will use expensive high-grade magnetic, significantly improved production cost.
Application number be 200510033577 patent application " a kind of method of clinkering anisotropic permanent ferrite through polymer bonding and modeling " disclose a kind of with ferrite powder with after the polymeric binder that accounts for raw material gross weight 0.1～3.0% is mixed, compression moulding, sintering obtain the method for anisotropy permanent-magnet ferrite.But this method only utilizes the oilness of polymeric binder itself to reach the purpose that reduces frictional coefficient between particle.Polymkeric substance has cohesiveness and oilness simultaneously under molten state, the two is conflicting.When temperature was low, the cohesiveness of polymkeric substance was better than oilness, and this is unfavorable for the orientation of magnetic particle.Along with the rising of temperature, distance becomes big between polymer molecule, and intermolecular frictional force reduces, the mobile enhancing, and lubrication is remarkable.But after temperature surpassed a certain value, because polymer bonding significantly reduces, its tack variation on ferrite powder, its oilness also reduced relatively.Therefore, use polymeric binder to be difficult to obtaining certain close-burning while separately, allow all magnetic particles orientations under the action of a magnetic field, cause the comprehensive magnetic property (maximum magnetic energy product) of the anisotropy permanent-magnet ferrite of this method preparation not reach the high level of wet moulding.
Summary of the invention
The objective of the invention is to overcome the shortcoming that exists in the prior art, a kind of environmental friendliness, magnetic property height, anisotropy method for preparing permanent magnetic ferrite that cost is low are provided.
Purpose of the present invention is achieved through the following technical solutions:
A kind of anisotropy method for preparing permanent magnetic ferrite, comprise ferrite powder mixed powder process, compression moulding, sintering that with polymeric binder wherein said polymeric binder contains the Zinic stearas of polymeric amide, polyethylene and fluorine-containing poly multipolymer and 25～40% (quality) of 60～75% (quality).
The Zinic stearas of the polymeric amide of described polymeric binder preferred 60～70% (quality), polyethylene and fluorine-containing poly multipolymer and 30～40% (quality).
Described polymeric amide, polyethylene and fluorine-containing poly multipolymer have the fusing point peak in 120～200 ℃ of scopes, the stable decomposition in 200～700 ℃ of scopes.
The particle diameter of described polymeric amide, polyethylene and fluorine-containing poly multipolymer＜14 μ m; The particle diameter of described Zinic stearas＜75 μ m.
Described Zinic stearas has layered crystal structure, and fusing point is about 130 ℃.The layered crystal structure of described Zinic stearas is outwards to be formed by stacking by Van der Waals force by the fatty acid radical terminal methyl; Because interlaminar action power is little, layer slides mutually easily with layer and throws off; Therefore Zinic stearas is pulverized easily, has soapy feeling.In described polymeric binder, add Zinic stearas, can significantly reduce the frictional coefficient of ferrite powder; And Zinic stearas can resolve into Zn, CO in sintering process
2And H
2O is eco-friendly material.
Described ferrite powder mixes powder process with polymeric binder, and polymeric binder accounts for 0.8～2.0% of mixture total mass, and the preferred polymers binding agent accounts for 1.2～1.4% of mixture total mass.
Described ferrite powder is the brilliant magneto-plumbite type ferrite powder of hexagonal MO6Fe
2O
3, wherein M is selected from a kind of element among Sr, Ba, the Pb; Preferred strontium ferrites powder SrFe
12O
19Ferrite powder can adopt regrind, oven dry, fragmentation, and granularity is preferably 0.9～1.1 μ m.
Described ferrite powder mixes powder process with polymeric binder, is with ferrite powder and polymeric binder thorough mixing, crosses 120～200 mesh sieves, and carries out dispersion treatment with mechanism and obtain mixture.
Described compression moulding is with above-mentioned ferrite powder and mixture heating up to 100～160 after polymeric binder is mixed powder process ℃, preferred 120～140 ℃; Simultaneously also with mold heated to 120～180 ℃, preferred 140～160 ℃; Described mixture is filled in the mould, is adding under 6～8kOe magnetic field, apply the above pressure compression moulding of 60MPa and obtain blank.
Described sintering is that slow cooling is come out of the stove, and obtains the anisotropy permanent-magnet ferrite with the sintering 0.5～2 hour in 1200～1280 ℃ of following air of the blank after the above-mentioned compression moulding.Preferred 1240～1260 ℃ of sintering temperature, preferred 1～1.5 hour of sintering time.
The present invention compared with prior art has following advantage and effect:
(1) cohesiveness of polymeric binder of the present invention and oilness are better, are the environmental friendliness materials, and harmless in process of production, environmental pollution is very little.
(2) the magnetic property height of the prepared anisotropy permanent-magnet ferrite of the present invention, approached the wet method level of magnetic at the same level, remanent magnetism reaches 96.9% of wet method product, maximum magnetic energy product reaches 93.8% of wet method product, and magnetic strength coercive force and HCJ all reach more than 100% of wet method product.
(3) use the present invention can reduce dry production anisotropy permanent-magnet ferrite production cost of products significantly.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed description, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) polymeric amide, polyethylene and the fluorine-containing poly multipolymer of 65% (quality) and the Zinic stearas thorough mixing of 35% (quality) are obtained polymeric binder, described polymeric amide, polyethylene and fluorine-containing poly multipolymer can be buied from market.
(2) with the brilliant magneto-plumbite type ferrite powder of hexagonal SrFe
12O
19, after regrind, oven dry, fragmentation, make its granularity at 0.9～1.1 μ m.
(3) will account for the above-mentioned polymeric binder and the above-mentioned ferrite powder thorough mixing 90min of mixture total mass 1.2%, cross 120～200 mesh sieves, and after carrying out dispersion treatment with mechanism.
(4) with the mixture heating up to 125 after the above-mentioned dispersion treatment ℃; , the mixture after the above-mentioned heating is filled in the heated mould simultaneously, is adding under 6～8kOe magnetic field, apply the above pressure compression moulding of 60MPa and obtain blank also with mold heated to 145 ℃.
(5) sintering is after 1～1.5 hour in 1240～1260 ℃ of following air with the blank after the above-mentioned compression moulding, and slow cooling is come out of the stove, and obtains anisotropy permanent-magnet ferrite product.
Embodiment 2
In the step 1, polymeric amide, polyethylene and the fluorine-containing poly multipolymer of 60% (quality) and the Zinic stearas thorough mixing of 40% (quality) are obtained polymeric binder; Other is with embodiment 1.
Embodiment 3:
In the step 1, polymeric amide, polyethylene and the fluorine-containing poly multipolymer of 70% (quality) and the Zinic stearas thorough mixing of 30% (quality) are obtained polymeric binder; Other is with embodiment 1.
Embodiment 4:
In the step 1, polymeric amide, polyethylene and the fluorine-containing poly multipolymer of 75% (quality) and the Zinic stearas thorough mixing of 25% (quality) are obtained polymeric binder; Other is with embodiment 1.
Embodiment 5:
In the step 3, the polymeric binder and the ferrite powder thorough mixing of mixture total mass 1.4% will be accounted for; Other is with embodiment 1.
Embodiment 6:
In the step 3, the polymeric binder and the ferrite powder thorough mixing of mixture total mass 1.8% will be accounted for; Other is with embodiment 1.
Embodiment 7:
In the step 4, with mixture heating up to 135 ℃, simultaneously also with mold heated to 155 ℃; Other is with embodiment 2.
Comparative example 1:
Wet method prepares the anisotropy permanent-magnet ferrite.The brilliant magneto-plumbite type ferrite powder of hexagonal SrFe that will be identical with embodiment 1
12O
19To become water content be about 37% through regrind to add water, and granularity is the slip of 1.06～1.11 μ m; Slip is put into mold cavity, under the alignment magnetic field of 6～8kOe, apply the above pressure compression moulding of 60MPa under the normal temperature; Sintering is after 1～1.5 hour in 1240～1260 ℃ of air, and slow cooling is come out of the stove.
Comparative example 2:
In the step 1, polymeric amide, polyethylene and the fluorine-containing poly multipolymer of 90% (quality) and the Zinic stearas thorough mixing of 10% (quality) are obtained polymeric binder; Other is with embodiment 1.
Comparative example 3:
In the step 1, polymeric amide, polyethylene and the fluorine-containing poly multipolymer of 50% (quality) and the Zinic stearas thorough mixing of 50% (quality) are obtained polymeric binder; Other is with embodiment 1.
Comparative example 4:
In the step 3, the polymeric binder and the ferrite powder thorough mixing of mixture total mass 0.4% will be accounted for; Other is with embodiment 1.
Comparative example 5:
In the step 4, with mixture heating up to 115 ℃, simultaneously also with mold heated to 135 ℃; Other is with embodiment 2.
Comparative example 6:
In the step 1, the polymeric binder of employing is the molybdenumdisulphide of polymeric amide, polyethylene and fluorine-containing poly multipolymer and 10% (quality) of 90% (quality); Other is with embodiment 1.
Comparative example 7:
In the step 1, the polymeric binder of employing is the molybdenumdisulphide of polymeric amide, polyethylene and fluorine-containing poly multipolymer and 20% (quality) of 80% (quality); Other is with embodiment 1.
Comparative example 8:
In the step 1, the polymeric binder of employing is the molybdenumdisulphide of polymeric amide, polyethylene and fluorine-containing poly multipolymer and 30% (quality) of 70% (quality); Other is with embodiment 1.
Comparative example 9:
In the step 1, the polymeric binder of employing is polymeric amide, polyethylene and fluorine-containing poly multipolymer; Other is with embodiment 1.
Comparative example 10:
In the step 1, the polymeric binder of employing is polymeric amide, polyethylene and the fluorine-containing poly multipolymer of 65% (quality), the Zinic stearas of 34% (quality), the molybdenumdisulphide of 1% (quality); Other is with embodiment 1.
Comparative example 11:
In the step 1, the polymeric binder of employing is polymeric amide, polyethylene and the fluorine-containing poly multipolymer of 65% (quality), the Zinic stearas of 33% (quality), the molybdenumdisulphide of 2% (quality); Other is with embodiment 1.
The magnetic property comparable situation of table 1 embodiment 1～7 and comparative example 1～11 obtained product
| Br (Gs) | H cb (Oe) | H cj (Oe) | (BH) max (MGOe) | |
| Embodiment 1 embodiment 2 embodiment 3 embodiment 4 embodiment 5 embodiment 6 embodiment 7 comparative examples 1 comparative example 2 comparative examples 3 comparative examples 4 comparative examples 5 comparative examples 6 comparative examples 7 comparative examples 8 comparative examples 9 comparative examples 10 comparative examples 11 | 3875 3847 3834 3780 3789 3796 3758 3999 3650 3717 3551 3613 3376 3126 3206 3645 3699 3617 | 2622 2620 2662 2714 2759 2822 2893 2605 2721 2560 2832 2924 2400 2206 2471 2762 2940 2994 | 2697 2733 2753 2837 2881 2975 2988 2692 2893 2717 3075 3053 2555 3006 2933 2933 3167 3250 | 3.64 3.58 3.53 3.44 3.44 3.40 3.46 3.88 3.19 3.30 2.94 3.05 2.63 1.73 2.24 3.14 3.28 3.11 |
The fundamental characteristics of permanent-magnet ferrite use always Br (remnant field), Hcb (magnetic strength coercive force), Hcj (HCJ) and (BH) four indexs of max (maximum magnetic energy product) represent that wherein (BH) max is basic index of weighing the permanent-magnet ferrite performance.From the result of table 1 as can be seen, the magnetic property of the anisotropy permanent-magnet ferrite of the present invention's preparation is higher.Wherein, the remanent magnetism of embodiment 1 sample has reached 96.9% of wet method product (comparative example 1), and maximum magnetic energy product reaches 93.8% of wet method product, and magnetic strength coercive force and HCJ all reach the level of wet method product.Compare with the binding agent that does not add Zinic stearas (comparative example 9), although the magnetic strength coercive force of embodiment 1 sample reduces by 5.3%, HCJ reduces by 8.8%, and remanent magnetism has improved 6.3%, maximum magnetic energy product has improved 15.9%, so the performance of comprehensive evaluation magnet is obviously to improve.
Claims (4)
1. anisotropy method for preparing permanent magnetic ferrite, comprise ferrite powder is mixed powder process, compression moulding, sintering with polymeric binder, it is characterized in that: described polymeric binder contains the Zinic stearas of polymeric amide, polyethylene and fluorine-containing poly multipolymer and 25～40 quality % of 60～75 quality %; Described ferrite powder mixes powder process with polymeric binder, and polymeric binder accounts for 0.8～2.0% of mixture total mass; Described compression moulding is with above-mentioned ferrite powder and mixture heating up to 100～160 after polymeric binder is mixed powder process ℃; Simultaneously also with mold heated to 120～180 ℃; Described mixture is filled in the mould, is adding under 6～8kOe magnetic field, apply the above pressure compression moulding of 60MPa and obtain blank; Described sintering is that slow cooling is come out of the stove, and obtains the anisotropy permanent-magnet ferrite with the sintering 0.5～2 hour in 1200～1280 ℃ of air of the blank after the described compression moulding.
2. anisotropy method for preparing permanent magnetic ferrite according to claim 1 is characterized in that: described polymeric binder contains the Zinic stearas of polymeric amide, polyethylene and fluorine-containing poly multipolymer and 30～40 quality % of 60～70 quality %.
3. anisotropy method for preparing permanent magnetic ferrite according to claim 1 is characterized in that: described ferrite powder mixes powder process with polymeric binder, and polymeric binder accounts for 1.2～1.4% of mixture total mass.
4. anisotropy method for preparing permanent magnetic ferrite according to claim 1 is characterized in that: described ferrite powder is the brilliant magneto-plumbite type ferrite powder of hexagonal MO.6Fe
2O
3, wherein M is selected from a kind of element among Sr, Ba, the Pb.
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| CNB2006100356986A CN100368344C (en) | 2006-05-30 | 2006-05-30 | Preparation process of anisotropic permanent magnetic ferrite |
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| CN105895359A (en) * | 2016-06-18 | 2016-08-24 | 丁文澜 | Method for producing anisotropism permanent-magnetic-ferrite multi-pole magnetic ring |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458118A (en) * | 2003-04-24 | 2003-11-26 | 哈尔滨工程大学 | Process for preparing nano permanent magnetic ferrite powder |
| CN1664964A (en) * | 2005-03-17 | 2005-09-07 | 华南理工大学 | Process for clinkering anisotropic permanent ferrite through polymer bonding and modeling |
| CN1770337A (en) * | 2005-09-16 | 2006-05-10 | 华南理工大学 | Method for preparing bonded permanent ferrite by direct injection forming after in-situ polymerization |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458118A (en) * | 2003-04-24 | 2003-11-26 | 哈尔滨工程大学 | Process for preparing nano permanent magnetic ferrite powder |
| CN1664964A (en) * | 2005-03-17 | 2005-09-07 | 华南理工大学 | Process for clinkering anisotropic permanent ferrite through polymer bonding and modeling |
| CN1770337A (en) * | 2005-09-16 | 2006-05-10 | 华南理工大学 | Method for preparing bonded permanent ferrite by direct injection forming after in-situ polymerization |
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