CN111933442A - Preparation method of oxide magnetic core for transformer - Google Patents
Preparation method of oxide magnetic core for transformer Download PDFInfo
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- CN111933442A CN111933442A CN202010809536.3A CN202010809536A CN111933442A CN 111933442 A CN111933442 A CN 111933442A CN 202010809536 A CN202010809536 A CN 202010809536A CN 111933442 A CN111933442 A CN 111933442A
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- oxide
- sintering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
Abstract
The invention relates to the technical field of magnetic core preparation, and discloses a preparation method of an oxide magnetic core for a transformer, which comprises the following steps: iron oxide (Fe) with the mass percentage of 51 to 55 percent2O3) 7 to 12 percent of zinc oxide (ZnO) and the balance of manganese oxide (Mn)3O4) And the raw materials of the trace additive are ball-milled into powder; powder and PVA binder are got to the title according to weight percentage, let in spray drying equipment and carry out the granulation, use the make-up machine shaping to become the ring sample, place the ring sample and sinter in the sintering equipment who has the binder removal device, at the in-process of sintering oxidation body magnetic core sample, the aspiration pump of binder removal device is to the inside draft that forms of sintering equipment furnace, the inside gas of furnace is taken out, the inside negative pressure environment that forms of furnace, under negative pressure, the inside and outside great pressure differential that forms of magnetic core, this pressure differential helps the discharge of gluey gas, the technological effect of the binder removal process in the control oxidation body magnetic core sample sintering process has been realized.
Description
Technical Field
The invention relates to the technical field of magnetic core preparation, in particular to a preparation method of an oxide magnetic core for a transformer.
Background
The core is an important component of the transformer, which is generally made of oxide magnetic material, and the oxide core is generally made of iron oxide (Fe)2O3) And one or more other metal (such as manganese, zinc, nickel, magnesium) oxide or carbonate compounds, by pressing, and then subjecting to 1300 deg.CAnd (4) sintering at high temperature, and machining to obtain the finished magnetic core meeting the application requirement.
In the forming stage of the oxide magnetic core manufacturing process, a certain amount of organic matters are used as a binder, so that the organic matters are removed before solid-phase reaction occurs, in the sintering and heating process of the oxide, the hearth pressure is generally kept at a positive pressure of 200 plus 1000Pa, the positive pressure inhibits the discharge of organic matter glue gas and impurities in the magnetic core to a certain extent, glue discharging is mainly carried out by prolonging the glue discharging time at present, the glue discharging time is prolonged, the power consumption is increased, the production period is prolonged, the production cost is increased, and the production efficiency is reduced.
Therefore, a suitable binder removal system is particularly important for the production of oxide cores.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of an oxide magnetic core for a transformer, which aims to solve the technical problem that the binder removal process in the sintering process cannot be controlled in the forming stage in the manufacturing process of the oxide magnetic core at present.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing an oxide magnetic core for a transformer, comprising the steps of:
the method comprises the following steps: preparation of the powder
Iron oxide (Fe) with the mass percentage of 51 to 55 percent2O3) 7 to 12 percent of zinc oxide (ZnO) and the balance of manganese oxide (Mn)3O4) Uniformly mixing the raw materials and the trace additive by a roller ball mill, calcining at 900-1000 ℃ for 2 hours, and ball-milling the raw materials and the trace additive into powder by the ball mill after calcining;
step two: preparation of oxide magnetic cores
Weighing 90% of powder and 10% of PVA adhesive according to the weight percentage, introducing the powder and the PVA adhesive into spray drying equipment for granulation, forming the powder and the PVA adhesive into a circular sample by using a forming machine, placing the circular sample into sintering equipment with a glue discharging device for sintering, controlling the sintering temperature at 1300 ℃, the negative pressure value at-200 Pa to-300 Pa, the oxygen partial pressure at 2% -5% and the sintering time at 5-7 h;
the glue discharging device of the sintering equipment comprises an air pump, a first connecting pipeline, a second connecting pipeline and a carbon molecular sieve;
the air inlet port of the first connecting pipeline of the glue discharging device is connected with an exhaust valve of the sintering equipment, and the exhaust valve of the sintering equipment is communicated with a hearth of the sintering equipment;
the exhaust port of the first connecting pipeline is communicated with the air inlet port of the second connecting pipeline through an air extracting pump;
the second connecting pipe is filled with carbon molecular sieve.
Further, in the first step, the rotating speed of the roller ball mill is 45r/min, and the ball milling time is 24 h.
Further, in the first step, after the calcination is finished, the powder with the granularity of 0.5-2.0 um is ball-milled by a ball mill.
Further, in the second step, the powder and the PVA adhesive are introduced into a spray drying device for granulation, and particles of 80-200 um are prepared.
Furthermore, the inner wall of the first connecting pipeline is coated with a titanium carbide-titanium nitride composite coating, wherein the titanium nitride is used as an interlayer and is inserted between the inner wall of the first connecting pipeline and the titanium carbide layer.
Furthermore, the inside of the first connecting pipeline is filled with a heat absorption sieve column close to the outlet of the exhaust port, air guide channels are uniformly distributed on the heat absorption sieve column, and the central shaft of each air guide channel and the central shaft of each heat absorption sieve column are arranged in parallel.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
in the process of sintering the oxide magnetic core sample, a suction pump of the glue discharging device forms suction force on the interior of a hearth of the sintering equipment, gas in the hearth is pumped out, a negative pressure environment is formed in the hearth, under the negative pressure, a large pressure difference is formed between the interior and the exterior of the magnetic core, the pressure difference is favorable for discharging the glue gas, and the technical effect of controlling the glue discharging process in the sintering process of the oxide magnetic core sample is achieved;
the discharged glue gas is separated by the carbon molecular sieve, so that the organic gas is prevented from being directly discharged into the atmosphere to cause environmental pollution;
the titanium carbide-titanium nitride composite coating is in direct contact with the inner wall of the first connecting pipeline by isolating high-temperature glue gas, so that the technical effect of preventing the high-temperature gas from damaging the first connecting pipeline is achieved;
the heat absorption sieve column can fully absorb the heat energy in the high-temperature glue gas while transmitting the glue gas through the gas guide channel, and the technical effects of reducing the temperature of the glue gas and preventing the high-temperature glue gas from damaging the air suction pump are achieved.
Drawings
FIG. 1 is a schematic diagram of a binder removal apparatus of a sintering apparatus used for sintering an oxide magnetic core sample;
fig. 2 is a cross-sectional view of the heat absorbing screen column of fig. 1.
The following are marked in the figure: 1-a sintering equipment hearth, 2-an air pump, 3-a first connecting pipeline, 301-a titanium carbide-titanium nitride composite coating, 302-a heat absorption sieve column, 4-a second connecting pipeline and 401-a carbon molecular sieve.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a method for preparing an oxide magnetic core for a transformer, comprising the steps of:
the method comprises the following steps: preparation of the powder
Mixing the materialsIron oxide (Fe) in an amount of 51%2O3) 12% of zinc oxide (ZnO), 31.9% of manganese oxide (Mn)3O4) 500PPM niobium pentoxide (Nb)2O5) 80PPM calcium oxide (CaO), 400PPM zirconium dioxide (ZrO)2) 1000PPM cobalt oxide (CoO), 700PPM vanadium pentoxide (V)2O5) 100PPM nickel oxide (NiO), 300PPM indium oxide (In)2O3) 10PPM of boron oxide (B)2O3) 30PPM of phosphorus pentoxide (P)2O5) The balance being tin oxide (SnO)2) The raw materials are uniformly mixed by a roller ball mill, the rotating speed of the roller ball mill is 45r/min, the ball milling time is 24 hours, then the raw materials are calcined at the temperature of 900 ℃, the calcining time is 2 hours, and after the calcining is finished, the raw materials are ball milled by the ball mill to powder with the granularity of 0.5 um;
wherein, 1 percent is 10000 PPM;
step two: preparation of oxide magnetic cores
Weighing 90% of powder and 10% of PVA adhesive according to weight percentage, introducing the powder and the PVA adhesive into spray drying equipment for granulation to prepare particles of 80um, forming the particles into a circular sample by using a forming machine, placing the circular sample into sintering equipment with a glue discharging device for sintering, controlling the sintering temperature at 1300 ℃, the negative pressure value at-300 Pa, the oxygen partial pressure at 2% and the sintering time at 7 h.
Example two:
a method for preparing an oxide magnetic core for a transformer, comprising the steps of:
the method comprises the following steps: preparation of the powder
Iron oxide (Fe) with the mass percentage of 55%2O3) 7% of zinc oxide (ZnO), 41.9% of manganese oxide (Mn)3O4) 80PPM niobium pentoxide (Nb)2O5) 700PPM calcium oxide (CaO), 80PPM zirconium dioxide (ZrO)2) 4500PPM cobalt oxide (CoO), 80PPM vanadium pentoxide (V)2O5) 3000PPM nickel oxide (NiO), 100PPM indium oxide (In)2O3)、30PBoron oxide (B) of PM2O3) 10PPM of phosphorus pentoxide (P)2O5) The balance being tin oxide (SnO)2) The raw materials are uniformly mixed by a roller ball mill, the rotating speed of the roller ball mill is 45r/min, the ball milling time is 24 hours, then the raw materials are calcined at the temperature of 1000 ℃, the calcining time is 2 hours, and after the calcining is finished, the raw materials are ball milled by the ball mill to powder with the granularity of 2.0 um;
step two: preparation of oxide magnetic cores
Weighing 90% of powder and 10% of PVA adhesive according to the weight percentage, introducing the powder and the PVA adhesive into spray drying equipment for granulation to prepare particles of 200um, forming the particles into a circular sample by using a forming machine, placing the circular sample into sintering equipment with a glue discharging device for sintering, controlling the sintering temperature at 1300 ℃, the negative pressure value at-200 Pa, the oxygen partial pressure at 5% and the sintering time at 5 h;
the sample is placed in a hearth 1 of sintering equipment of the sintering equipment for sintering, in the sintering process, a glue discharging device of the sintering equipment forms suction force on the interior of the hearth 1 of the sintering equipment, gas in the hearth is pumped out, a negative pressure environment is formed in the hearth, the negative pressure value in the hearth is controlled to be-200 Pa to-300 Pa, under the negative pressure of 200Pa to 300Pa, a large pressure difference is formed between the interior and the exterior of a magnetic core, the pressure difference is favorable for discharging glue gas, and the discharged glue gas is purified through the glue discharging device, so that the environmental pollution caused by the fact that organic gas is directly discharged into the atmosphere is avoided;
as shown in fig. 1, the glue discharging device of the sintering equipment used for sintering the oxide magnetic core sample comprises an air pump 2, a first connecting pipeline 3, a titanium carbide-titanium nitride composite coating 301, a heat absorption sieve column 302, a second connecting pipeline 4 and a carbon molecular sieve 401;
an air inlet port of a first connecting pipeline 3 of the glue discharging device is connected with an exhaust valve of the sintering equipment, and the exhaust valve of the sintering equipment is communicated with a hearth 1 of the sintering equipment;
the exhaust port of the first connecting pipeline 3 is communicated with the air inlet port of the second connecting pipeline 4 through the air extracting pump 2;
a titanium carbide-titanium nitride composite coating 301 is coated on the inner wall of the first connecting pipe 3, wherein titanium nitride with good thermal stability is used as an interlayer and is inserted between the inner wall of the first connecting pipe 3 and the titanium carbide layer;
a heat absorption sieve column 302 is filled in the first connecting pipeline 3 near the exhaust port, as shown in fig. 2, air guide channels are uniformly distributed on the heat absorption sieve column 302, and the central axes of the air guide channels and the central axis of the heat absorption sieve column 302 are arranged in parallel;
the titanium carbide-titanium nitride composite coating 301 has the technical effect of preventing high-temperature gas from damaging the first connecting pipeline 3 by isolating the high-temperature glue gas from directly contacting the inner wall of the first connecting pipeline 3;
the heat absorption sieve column 302 can fully absorb the heat energy in the high-temperature glue gas while transmitting the glue gas through the gas guide channel, and has the technical effects of reducing the temperature of the glue gas and preventing the high-temperature glue gas from damaging the air suction pump 2;
the carbon molecular sieve 401 is filled in the second connecting pipeline 4, the carbon molecular sieve 401 separates organic gas from carbon dioxide and water molecules in the glue gas, the carbon dioxide and the water molecules can be directly discharged into the atmosphere, and the separated organic gas is recycled;
when arranging the glue, suction pump 2 is to 1 inside draft that forms of sintering equipment furnace, and the inside gas of furnace is taken out, and the inside negative pressure environment that forms of furnace, under negative pressure, the inside and outside great pressure differential that forms of magnetic core, this pressure differential help gluing the discharge of gas, and exhaust gluey gas passes through carbon molecular sieve 401 and carries out the separation processing, has avoided organic gas directly to discharge into in the atmosphere, causes environmental pollution.
And (3) performance testing:
the performance of the circular epoxy body magnetic core prepared in the above embodiment was tested by using an impedance analyzer and a soft magnetic alternating current B-H tester at a temperature of 21.9-22.6℃ and a humidity of 52.1-52.9% according to GB/T28869.1-2012, and the specific test items were as follows: initial permeability μiPower loss PCVSaturation magnetic flux density BsResidual magnetic flux density BrCoercive force HCCurie temperature of
Resistivity rho*And density d, the test results are shown in the following tables 1 to 4.
TABLE 1
TABLE 2
TABLE 3
TABLE 4
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A method for preparing an oxide magnetic core for a transformer, comprising the steps of:
the method comprises the following steps: preparation of the powder
Iron oxide (Fe) with the mass percentage of 51 to 55 percent2O3）、7%～12% of zinc oxide (ZnO), and the balance of manganese oxide (Mn)3O4) Uniformly mixing the raw materials and the trace additive by a roller ball mill, calcining at 900-1000 ℃ for 2 hours, and ball-milling the raw materials and the trace additive into powder by the ball mill after calcining;
step two: preparation of oxide magnetic cores
Weighing 90% of powder and 10% of PVA adhesive according to the weight percentage, introducing the powder and the PVA adhesive into spray drying equipment for granulation, forming the powder and the PVA adhesive into a circular sample by using a forming machine, placing the circular sample into sintering equipment with a glue discharging device for sintering, controlling the sintering temperature at 1300 ℃, the negative pressure value at-200 Pa to-300 Pa, the oxygen partial pressure at 2% -5% and the sintering time at 5-7 h;
the glue discharging device of the sintering equipment comprises an air extracting pump (2), a first connecting pipeline (3), a second connecting pipeline (4) and a carbon molecular sieve (401);
the air inlet port of the first connecting pipeline (3) of the glue discharging device is connected with an exhaust valve of the sintering equipment, and the exhaust valve of the sintering equipment is communicated with a hearth (1) of the sintering equipment;
the exhaust port of the first connecting pipeline (3) is communicated with the air inlet port of the second connecting pipeline (4) through the air extracting pump (2);
the second connecting pipe (4) is filled with a carbon molecular sieve (401).
2. The method for preparing an oxide magnetic core for a transformer according to claim 1, wherein in the first step, the rotation speed of the ball tumbling mill is 45r/min, and the ball milling time is 24 h.
3. The method of claim 2, wherein in the first step, the powder with a particle size of 0.5um to 2.0um is ball milled by a ball mill after calcination.
4. The method of claim 3, wherein in the second step, the powder and the PVA binder are granulated by a spray drying apparatus to obtain particles of 80-200 um.
5. Method for the production of an oxide core for a transformer according to claim 4, wherein said first connecting duct (3) is coated on its inner wall with a titanium carbide-titanium nitride composite coating (301) with titanium nitride as an interlayer interposed between the inner wall of the first connecting duct (3) and the titanium carbide layer.
6. The method for preparing an oxide core for a transformer according to claim 5, wherein the inside of the first connecting pipe (3) is filled with a heat absorbing sieve column (302) near the exhaust port, air guide channels are uniformly distributed on the heat absorbing sieve column (302), and the central axes of the air guide channels and the heat absorbing sieve column (302) are arranged in parallel.
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| CN202010809536.3A CN111933442A (en) | 2020-08-13 | 2020-08-13 | Preparation method of oxide magnetic core for transformer |
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| CN101183585A (en) * | 2007-09-26 | 2008-05-21 | 广东风华高新科技股份有限公司 | MnZn ferrite material and method of manufacturing the magnetic core |
| CN201096465Y (en) * | 2007-09-29 | 2008-08-06 | 中冶京诚工程技术有限公司 | Composite honeycomb heat accumulator |
| CN103884179A (en) * | 2013-11-13 | 2014-06-25 | 山东嘉诺电子有限公司 | Negative-pressure soft magnetic ferrite core sintering device with glue and oxygen discharging function of bell kiln |
| CN104946995A (en) * | 2015-05-17 | 2015-09-30 | 王华美 | High-temperature-resistant exhaust valve for car engine |
| CN205570067U (en) * | 2016-03-09 | 2016-09-14 | 安徽理工大学 | Simple and easy laboratory exhaust purification processing system |
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- 2020-08-13 CN CN202010809536.3A patent/CN111933442A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101183585A (en) * | 2007-09-26 | 2008-05-21 | 广东风华高新科技股份有限公司 | MnZn ferrite material and method of manufacturing the magnetic core |
| CN201096465Y (en) * | 2007-09-29 | 2008-08-06 | 中冶京诚工程技术有限公司 | Composite honeycomb heat accumulator |
| CN103884179A (en) * | 2013-11-13 | 2014-06-25 | 山东嘉诺电子有限公司 | Negative-pressure soft magnetic ferrite core sintering device with glue and oxygen discharging function of bell kiln |
| CN104946995A (en) * | 2015-05-17 | 2015-09-30 | 王华美 | High-temperature-resistant exhaust valve for car engine |
| CN205570067U (en) * | 2016-03-09 | 2016-09-14 | 安徽理工大学 | Simple and easy laboratory exhaust purification processing system |
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Application publication date: 20201113 |