CN105924147A - Preparation method for powder material used for large-sized soft magnetic ferrite - Google Patents
Preparation method for powder material used for large-sized soft magnetic ferrite Download PDFInfo
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- CN105924147A CN105924147A CN201610277671.1A CN201610277671A CN105924147A CN 105924147 A CN105924147 A CN 105924147A CN 201610277671 A CN201610277671 A CN 201610277671A CN 105924147 A CN105924147 A CN 105924147A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
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Abstract
The invention discloses a preparation method for a powder material used for large-sized soft magnetic ferrite. The preparation method comprises the following steps: (1) weighing Fe2O3, ZnO and MnO according to a proportion of molar content, then placing the components into a strongly-mixing vibration mill, and carrying out mechanical mixing so as to obtain a mixed powder material; (2) placing the mixed powder material into a pre-sintering furnace, carrying out pre-sintering, and carrying out cooling; (3) adding a dispersant, calcium carbonate, zirconium oxide and niobium oxide into the pre-sintered mixed powder material, then adding water, and carrying out sanding so as to obtain a sanded slurry; and (4) adding PVA into the sanded slurry, carrying out mixing under stirring, and carrying out spray granulation. The preparation method provided by the invention optimizes and improves the components and a sintering process of the powder material, reduces the addition amount of PVA, effectively solves the problem of cracking during preparation of a magnetic core, and shortens a dumping period of the magnetic core in the process of sintering.
Description
Technical field
The present invention relates to soft magnetic ferrite technical field, especially relate to a kind of powder preparation method for big specification soft magnetic ferrite.
Background technology
Soft magnetic ferrite is because its resistivity is high, high-frequency loss is low, it is variously-shaped to be processed into, high chemical stability, cost are cheap and be widely used in the fields such as mains transformer, Telecommunication Transformers, CRT deflection coil, choke coil, wave filter.And along with the development in epoch, newly-designed appearance, soft magnetic ferrite performance is had higher requirement by electronic equipment, because being limited to performance and the cost of soft magnetic ferrite, generally requiring and obtaining bigger by the specifications design of soft magnetic device.
The soft magnetic core of big specification, two problems of existence when making: (1) difficult forming: when suppressing the magnetic core of big specification, generally require higher briquetting pressure to reach more satisfactory compact density, bigger to mould and moulding press all loads；(2) sintering period is long: because the change of device specification is big, magnetic core is easier to cracking, needs to add more glue, and glue quantity increases, and the binder removal phase in sintering process needs to extend, and more extends the sintering period.Therefore exploitation is suitable for making the powder body of the soft magnetic core of big specification is the current task of top priority.
Summary of the invention
The present invention is to solve the powder body of prior art difficult forming when making the soft magnetic core of big specification, problem easy to crack, provide a kind of processing step simple, workable, preparation cost is low, the magnet ring binder removal sintering period can be shortened, and effectively solve soft magnetic ferrite powder preparation method for big specification soft magnetic ferrite of problem of Cracking in manufacturing process.
To achieve these goals, the present invention is by the following technical solutions:
A kind of powder preparation method for big specification soft magnetic ferrite of the present invention, comprises the following steps:
(1) by 50 ~ 52%Fe2O3, 9.5 ~ 10% ZnO, surplus is after the molar content of MnO weighs each component, each component is put into strong mixed vibrating ball-mill and carries out mechanical mixture, obtain mixed powder.Powder formulation is optimized improvement, to reduce the generation of cracking in magnetic core sintering process.
(2) mixed powder is placed in pre-burning stove, with 860 ~ 890 DEG C of pre-burning 2 ~ 3h, is cooled to room temperature.
(3), on the basis of the mixed powder quality after pre-burning, the mixed powder after pre-burning adds 0.16 ~ 0.22% dispersant, 600 ~ 620ppm calcium carbonate, 200 ~ 220ppm zirconium oxide, 200 ~ 220ppm niobium oxide, adds water after mix homogeneously and carry out sand milling, obtain sand milling slurry.
(4) the mixed powder quality 0.65 ~ 0.9%PVA after being incorporated as pre-burning in sand milling slurry, mist projection granulating after stirring.In the present invention, inventor is through constantly test, and the addition of PVA must be strict controlled in the mixed powder quality 0.65 ~ 0.9% after pre-burning, exceedes this scope, and prepared magnetic core is easy to crack in sintering process, or sintering time need to be greatly prolonged.
As preferably, in step (2), pre-burning heating rate is 2 ~ 5 DEG C/min.
As preferably, in step (3), described dispersant is ammonium citrate.
As preferably, in step (3), sand milling to slurry particle diameter is 1.2 ~ 1.3 μm.
As preferably, in step (4), the pine dress ratio of mist projection granulating controls at 1.38 ~ 1.55g/cm3.The molding of pine dress comparison powder is extremely important, by controlling pine dress ratio in the present invention, to avoid green density uneven, it is ensured that the intensity of green compact, it is to avoid when green compact compacting and sintering, cracking cracks.
Therefore, there is advantages that
(1) powder batching and sintering process are optimized improvement, and strictly control the pine dress ratio of powder, jointly coordinate to efficiently solve the problem that magnetic core ftractures in the preparation；
(2) decrease the addition of PVA, under ensureing the indehiscent premise of magnetic core, shorten the magnetic core binder removal phase in sintering process, thus shorten the magnetic core sintering period.
Detailed description of the invention
Below by the present invention will be further described with detailed description of the invention.
In the present invention, if not refering in particular to, all percentage ratios are unit of weight, all devices and raw material and are all commercially available or the industry is conventional, the method in following embodiment, if no special instructions, are this area conventional method.
Embodiment 1
(1) 50%Fe is pressed2O3, 9.5% ZnO, surplus is after the molar content of MnO weighs each component, each component is put into strong mixed vibrating ball-mill and carries out mechanical mixture, obtain mixed powder；
(2) mixed powder is placed in pre-burning stove, is warming up to 860 DEG C of pre-burning 2h with the heating rate of 2 DEG C/min, is cooled to room temperature；
(3), on the basis of the mixed powder quality after pre-burning, the mixed powder after pre-burning adds 0.16% dispersant ammonium citrate, 600ppm calcium carbonate, 200ppm zirconium oxide, 200ppm niobium oxide, adding water after mix homogeneously, to carry out sand milling to slurry particle diameter be 1.2 μm, obtains sand milling slurry；
(4) the mixed powder quality 0.65 ~ 0.9%PVA after being incorporated as pre-burning in sand milling slurry, mist projection granulating after stirring, control pine dress ratio during mist projection granulating at 1.38g/cm3。
Embodiment 2
(1) 52%Fe is pressed2O3, 10% ZnO, surplus is after the molar content of MnO weighs each component, each component is put into strong mixed vibrating ball-mill and carries out mechanical mixture, obtain mixed powder；
(2) mixed powder is placed in pre-burning stove, is warming up to 890 DEG C of pre-burning 3h with the heating rate of 5 DEG C/min, is cooled to room temperature；
(3), on the basis of the mixed powder quality after pre-burning, the mixed powder after pre-burning adds 0.22% dispersant ammonium citrate, 620ppm calcium carbonate, 220ppm zirconium oxide, 220ppm niobium oxide, adding water after mix homogeneously, to carry out sand milling to slurry particle diameter be 1.2 ~ 1.3 μm, obtains sand milling slurry；
(4) mixed powder quality 0.9%PVA after being incorporated as pre-burning in sand milling slurry, mist projection granulating after stirring, control pine dress ratio during mist projection granulating at 1.55g/cm3。
Embodiment 3
(1) 51%Fe is pressed2O3, 9.8% ZnO, surplus is after the molar content of MnO weighs each component, each component is put into strong mixed vibrating ball-mill and carries out mechanical mixture, obtain mixed powder；
(2) mixed powder is placed in pre-burning stove, is warming up to 870 DEG C of pre-burning 2.5h with the heating rate of 3 DEG C/min, is cooled to room temperature；
(3), on the basis of the mixed powder quality after pre-burning, the mixed powder after pre-burning adds 0.2% dispersant ammonium citrate, 610ppm calcium carbonate, 210ppm zirconium oxide, 210ppm niobium oxide, adding water after mix homogeneously, to carry out sand milling to slurry particle diameter be 1.25 μm, obtains sand milling slurry；
(4) mixed powder quality 0.8%PVA after being incorporated as pre-burning in sand milling slurry, mist projection granulating after stirring, control pine dress ratio during mist projection granulating at 1.42g/cm3。
The powder that the various embodiments described above prepare is suppressed on press the magnet ring of 80*40*15mm, the magnet ring after compacting is sintered again.
Magnet ring after compacting is separately immersed in kerosene, see blister formation, if a large amount of bubble occurs, then there is molding cracking, magnet ring after sintering judges whether cracking by range estimation, and result is: the magnet ring after the powder pressing suppressed by each embodiment and after sintering is all without cracking situation.It can thus be appreciated that the powder that the present invention prepares can effectively solve soft magnetic ferrite problem of Cracking in manufacturing process, it is worthy of popularization.
Embodiment described above is the one preferably scheme of the present invention, and the present invention not makees any pro forma restriction, also has other variant and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (5)
1. the powder preparation method for big specification soft magnetic ferrite, it is characterised in that comprise the following steps:
(1) by 50 ~ 52%Fe2O3, 9.5 ~ 10% ZnO, surplus is after the molar content of MnO weighs each component, each component is put into strong mixed vibrating ball-mill and carries out mechanical mixture, obtain mixed powder；
(2) mixed powder is placed in pre-burning stove, with 860 ~ 890 DEG C of pre-burning 2 ~ 3h, is cooled to room temperature；
(3), on the basis of the mixed powder quality after pre-burning, the mixed powder after pre-burning adds 0.16 ~ 0.22% dispersant, 600 ~ 620ppm calcium carbonate, 200 ~ 220ppm zirconium oxide, 200 ~ 220ppm niobium oxide, adds water after mix homogeneously and carry out sand milling, obtain sand milling slurry；
(4) the mixed powder quality 0.65 ~ 0.9%PVA after being incorporated as pre-burning in sand milling slurry, mist projection granulating after stirring.
A kind of powder preparation method for big specification soft magnetic ferrite the most according to claim 1, it is characterised in that in step (2), pre-burning heating rate is 2 ~ 5 DEG C/min.
A kind of powder preparation method for big specification soft magnetic ferrite the most according to claim 1, it is characterised in that in step (3), described dispersant is ammonium citrate.
A kind of powder preparation method for big specification soft magnetic ferrite the most according to claim 1, it is characterised in that in step (3), sand milling to slurry particle diameter is 1.2 ~ 1.3 μm.
A kind of powder preparation method for big specification soft magnetic ferrite the most according to claim 1, it is characterised in that in step (4), the pine dress ratio of mist projection granulating controls at 1.38 ~ 1.55g/cm3。
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| CN201610277671.1A CN105924147A (en) | 2016-04-28 | 2016-04-28 | Preparation method for powder material used for large-sized soft magnetic ferrite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111863367A (en) * | 2020-08-04 | 2020-10-30 | 山东东泰方思电子有限公司 | Method for manufacturing manganese-zinc ferrite magnetic core |
| CN113402284A (en) * | 2021-07-27 | 2021-09-17 | 横店集团东磁股份有限公司 | Method for solving sintering cracking of soft magnetic ferrite |
| CN113979755A (en) * | 2021-11-04 | 2022-01-28 | 无锡斯贝尔磁性材料有限公司 | Process control method for improving powder apparent density ratio of MnZn ferrite powder |
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| CN1686927A (en) * | 2005-03-21 | 2005-10-26 | 乳源瑶族自治县东阳光实业发展有限公司 | Higher magnetic permcability lowloss ferritc in manganese zinc series and preparation method thereof |
| CN101004961A (en) * | 2006-12-11 | 2007-07-25 | 电子科技大学 | Process for preparing high frequency high power ferrite material |
| CN101921102A (en) * | 2010-07-09 | 2010-12-22 | 广东风华高新科技股份有限公司 | Method for preparing high-precision and high-stability temperature control manganese zinc (Mn-Zn) soft magnetic ferrite material and magnetic core product obtained thereby |
| CN104086167A (en) * | 2014-06-12 | 2014-10-08 | 天长市中德电子有限公司 | Soft magnetic ferrite material and preparation process thereof |
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2016
- 2016-04-28 CN CN201610277671.1A patent/CN105924147A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1686927A (en) * | 2005-03-21 | 2005-10-26 | 乳源瑶族自治县东阳光实业发展有限公司 | Higher magnetic permcability lowloss ferritc in manganese zinc series and preparation method thereof |
| CN101004961A (en) * | 2006-12-11 | 2007-07-25 | 电子科技大学 | Process for preparing high frequency high power ferrite material |
| CN101921102A (en) * | 2010-07-09 | 2010-12-22 | 广东风华高新科技股份有限公司 | Method for preparing high-precision and high-stability temperature control manganese zinc (Mn-Zn) soft magnetic ferrite material and magnetic core product obtained thereby |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111863367A (en) * | 2020-08-04 | 2020-10-30 | 山东东泰方思电子有限公司 | Method for manufacturing manganese-zinc ferrite magnetic core |
| CN113402284A (en) * | 2021-07-27 | 2021-09-17 | 横店集团东磁股份有限公司 | Method for solving sintering cracking of soft magnetic ferrite |
| CN113979755A (en) * | 2021-11-04 | 2022-01-28 | 无锡斯贝尔磁性材料有限公司 | Process control method for improving powder apparent density ratio of MnZn ferrite powder |
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Application publication date: 20160907 |