CN1812019A - Low-temperature sintering production technology for magnetic ferrite and inductive material - Google Patents
Low-temperature sintering production technology for magnetic ferrite and inductive material Download PDFInfo
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- CN1812019A CN1812019A CN 200510135937 CN200510135937A CN1812019A CN 1812019 A CN1812019 A CN 1812019A CN 200510135937 CN200510135937 CN 200510135937 CN 200510135937 A CN200510135937 A CN 200510135937A CN 1812019 A CN1812019 A CN 1812019A
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Abstract
This method provides a kind of manufacture method of low-temperature sintering magnetic ferrite material using on electric induction coil. To use a kind of or various kinds of mixture solution metal salt (the salt is soluble salt of metal such as iron, nickel, manganese, copper, zinc, barium, cobalt, strontium and magnesium) to react with soluble oxalate solution and generate metal oxalate deposition. After filtration, washing and separating, heating and decompose to generate even particle diameter ferrite powder under protection gas. Add an amount of addition agents (such as compounds of calcium, silicon, bismuth or boron) to the powder. Adjust sintering temperature and electromagnetic property of sintering body through adjusting the components and contents of addition agents. Put the powder in the mould and press to form shape. Keep under protection gas and temperature of 800-1000DEG C for 1-20 hours and sintering to make the sintering body.
Description
Technical field
The present invention relates to the ferrite powder low-temperature sintering technology.Be particularly related to and be applicable to Fe
3O
4, MnZn, NiZn, MgZn and BaOnFe
2O
3, PbOnFe
2O
3, SrOnFe
2O
3Etc. the low-temperature sintering of various magnetic ferrites, especially be applicable to the ferritic low-temperature sinterings of stack-up type inductance coil such as MnCuZn, NiCuZn, MgCuZn.
Background technology
In the magnetic material development history, before the twenties in 20th century, nearly all be the metal based material, and reach practicability at first.But, along with the expansion of the market demand from electric power to the communication, press for be suitable for working under the higher frequency, resistivity height, soft magnetic material that eddy current loss is lower.In order to adapt to this requirement, ferrite (is the oxidate magnetic material of main component with the iron oxide) arises at the historic moment, and reaches practicability.Tokyo Institute of Technology in 1931 adds after rattan, the Wu Jing invention novel magnetic body, and oxide magnetic compact (ceramic-like magnetic) begins to occur.The soft magnetism compound of practicability mainly is an oxide magnetic compact, generally is called soft magnetic ferrite.
Soft magnetic ferrite is widely used in spacious and comfortable transformer, noise filter, communication with fields such as transformers.Because these purposes are relevant with signal processing, usefulness is the characteristic of ferrite under low-intensity magnetic field mostly.In recent years, it is more and more that ferrite is used for the situation of high-intensity magnetic field, thus the ferritic magnetic of MnZn that saturated magnetic flux density is the highest in the soft magnet body brought into play, use more and morely as the magnetic core of power transformer and choking-winding etc.Saturated magnetic flux density height is most important condition in these purposes.Particularly arrive the high frequency band territories of counting megahertz at thousands of hertz, because the increase of eddy current loss, so can not use metal materials such as silicon steel, molybdenum permalloy, and can only adopt MnZn ferrite etc.Such ferrite is suitable for preparing the electronic component of miniaturization power supply and high-frequency work condition.Arriving in the so-called radio frequency band territory below hundreds of megahertzes more than hundreds of kilo hertzs, mainly use NiZn and NiCuZn ferrite.In this frequency band territory.It is low-loss that first of magnetic material is required.Along with the increase of frequency, the particularly residual loss increase of eddy current loss is very fast.Ferritic resistivity height such as NiZn, eddy current loss is little.It mainly is the core material that signal processing is used that main application in this frequency band territory has intermediate frequency transformer used in a large amount of electronic equipments such as radio, TV, VTR, digital camera and Digital Video, inductor, antenna etc.In general, be that winding around constitutes transformer or inductor on sintered body, therefore be difficult to realize miniaturization.This year, along with the development of electronic equipment, utilize thick film technology to digitlization, miniaturization, lightness, be the lamination type components and parts with coil arrangement at the inner once-firing of ferrite, alternative original various electric elements.
Laminate sheet-like ferrite device and composite laminate type device, because of its volume is little, the unfailing performance height, characteristics such as anti-electromagnetic interference have been used for various electric elements.The common manufacture method of laminate sheet-like ferrite device is: utilize ferrite powder is made substrate, low-temperature sintering becomes sintered body, makes internal electrode and compound stalk forming at its surperficial distribution then, carries out low-temperature sintering again.Prepare electrode at last in the formed body end and constitute ceramic lamination inductance coil.Use silver-colored or silver-colored alloy proper in order to reduce the resistivity internal electrode.Cause sintering temperature must be lower than the fusing point of the alloy of silver or silver.Therefore, in order to obtain the cascade type ferrite device of high density, high characteristic, the fusing point that ferritic sintering temperature also must be lower than the alloy of silver or silver becomes the key for preparing the laminate sheet-like ferrite device.
Summary of the invention
Therefore, the objective of the invention is, address the above problem and provide the manufacture method of a kind of inductance coil with the low-temperature sintering magnetic ferrites materials, by changing the ferrite component content, reduce the particle size of synthetic powder, improve the surface activity energy, add an amount of additive, thereby reach the reduction sintering temperature, improve the magnetic characteristic and the mechanical strength of magnetic sintered body.The ferrite lamination inductance coil that utilizes the present invention to prepare has characteristics such as resistivity height, mechanical strength height, electromagnetic performance be good.
In order to address the above problem, the inventor by changing the ferrite component content, reduces the particle size of synthetic powder through discovering, improves the surface activity energy, adds an amount of additive, thereby reduces sintering temperature, reaches purpose of the present invention.
Promptly, the present invention is the manufacture method of inductance coil with the low-temperature sintering magnetic ferrites materials, (this salt is at first to utilize one or more slaines, metal soluble salt classes such as iron, nickel, manganese, copper, zinc, barium, cobalt, strontium and magnesium) the mixed solution and the solution of solubility oxalates react, and generate the metal oxalate precipitation that is not soluted in water.Filter, wash, separate back heating and decomposition under protection gas and prepare the uniform ferrite micropowder of particle size distribution.In micro mist, add an amount of additive (additive is calcic, silicon, bismuth or boron compound) and reach the sintering temperature of adjusting sintered body and the effect of electromagnetic property by composition and the content of regulating additive.This powder is put into the mould extrusion forming, and under protection gas, the 800-1000 degree kept 1-20 hour down, and sintering is made sintered body.
The described sintered body in aspect of the present invention is characterized in that, the Curie temperature of sintered body is the 300-600 degree.
The present invention prepares magnetic ferrite powder, sintered body and ferrite lamination inductance coil by the following method: (this oxalate precipitation is the mixture more than a kind or 2 kinds in iron and nickel, manganese, copper, zinc, barium, cobalt, strontium and the magnesium at first to utilize the synthetic metal oxalate precipitation of chemical coprecipitation; wherein iron concentration is 47mol%-50mol%); decompression; filter; washing; separate the back and under protection gas, be heated to the 300-700 degree; it is little to keep 10-120min to make ferric oxalate salt decompose the preparation particle, the uniform ferrite micropowder of particle diameter.Add an amount of additive (additive is a calcic, silicon, bismuth, boron compound) then in the micro mist.Reach the sintering temperature of adjusting sintered body and the effect of electromagnetic property by composition and the content of regulating additive.After this powder put into mould pressurization 0.5MPa-2MPa moulding, under protection gas, the 800-1000 degree kept 1-20 hour down, and low-temperature sintering is made sintered body.
Description of drawings
Fig. 1. for utilizing the TG_DTA curve chart of the prepared ferric oxalate that goes out of the present invention.
Fig. 2. for utilizing the XRD inflection diffraction pattern and the stereoscan photograph of the prepared magnetic ferrite powder that goes out of the present invention.
Fig. 3. be the thermal contraction curve (TMA) of sintered body among the present invention.
Fig. 4. for utilizing the prepared ferritic saturation magnetisation value curve that goes out of the present invention.
Fig. 5. for utilizing the prepared ferritic three-point bending mechanical strength curve that goes out of the present invention.
Fig. 6. for utilizing the prepared ferritic electromicroscopic photograph of MnCuZn that goes out of the present invention.
Fig. 7. prepare the ferritic high frequency permeability curcve of MnCuZn for utilizing the present invention
Fig. 8. prepare the ferritic highfrequency figure of merit curve of MnCuZn for utilizing the present invention.
Fig. 9. for utilizing the NiCuZn ferrite frequency that the present invention 950 degree sintering prepare and the relation curve of magnetic susceptibility.
Figure 10. for utilizing the prepared ferrite sintered temperature of NiCuZn that goes out of the present invention and the relation curve of magnetic susceptibility.
Embodiment
The present invention is applicable to the low-temperature sintering of various Ferrite Materials, is applicable to various ferritic sintering, as Fe
3O
4, BaZnFe
6Ou, BaO6Fe
2O
3, particularly be applicable to MnZn, NiZn, MgZn, MnCuZn, NiCuZn, the ferritic low-temperature sinterings of stack-up type inductance coil such as MgCuZn.
Below, be described more specifically the present invention according to embodiment.But the present invention is not limited in these embodiment.
Table 1
| The pH value | Ferric oxalate particle size (μ m) | Ferriferrous oxide particles size (μ m) | Reference area (the m of ferriferrous oxide particles 2/g) | The saturation magnetisation value of ferroferric oxide powder (emu/g) |
| 3 | 0.3 | 0.1 | 5 | 47 |
| 7 | 0.7 | 0.5 | 15 | 62 |
| 12 | 1.5 | 1.0 | 30 | 75 |
Common magnetic ferrites Fe
3O
4Preparation
At first make certain density Fe by preset blending ratio
2+And Fe
3+Solution is measured a certain amount of test solution by ferritic composition, evenly mixes and is preheated to uniform temperature, and crystalline powder is dissolved fully; Take by weighing a certain amount of oxalic acid ammonia by the coprecipitation reaction proportioning simultaneously and be made into certain density solution; Two kinds of solution are added in the 100ml aqueous solution simultaneously then, and stir 1h.Fully after the reaction, stop to stir, be cooled to room temperature.Precipitation is filtered, and yellow ferric oxalate powder is made in washing after the drying.By control reaction system pH value, thereby the particle size of may command ferric oxalate and by control ferric oxalate particle size reach control Fe
3O
4The particle size at magnetic micro-powder end is as shown in table 1.This ferric oxalate is Fe
3O
4The presoma of magnetic sintered body.
Secondly under carbon-dioxide protecting gas ferric oxalate is put into quartz ampoule, keep taking out from electric furnace behind the 1h at 500 ℃, water quenching is prepared Fe
3O
4Magnetic micro-powder.
Table 2
| Sintering temperature (℃) | Particle size (μ m) | Saturation magnetisation value (emu/g) | Density (the g/cm of sintered body 2) | The sintered body Curie temperature (℃) | The three-point bending strength of sintered body (MPa) |
| 900 | 1 | 62 | 4.2 | 440 | 250 |
| 1000 | 3 | 74 | 5.1 | 520 | 350 |
| 1100 | 5 | 90 | 5.8 | 580 | 400 |
Add an amount of boride powder (also can be calcium, silicon or bismuth compound, as follows) at last in this micro mist, for example 0-1mass% makes mixed-powder.Mixed-powder is filled in the mould, makes formed body after the pressurization.Keep 5 hours sintering to prepare sintered body in 900-1100 ℃ in carbon-dioxide protecting gas.It is as shown in table 2 that boride adds the various physical characteristics that prepare ferrite cemented body in right amount.Use electron microscope (SEM) that its particle size is observed, particle size range is 1-5 μ m.Utilize oscillating mode magnetic susceptibility determinator (VSM) that it has been carried out the magnetic properties evaluation, this sintered body saturation magnetisation value is 62-90emu/g.Use densitometer that the density of this sintered body has been carried out measuring density and be 4.2-5.8g/cm
2, the mechanical three-point bending strength to this material has carried out evaluation 250-400MPa at last.
Embodiment 2
Make certain density Ba by preset blending ratio
2+, Zn
2+, Fe
2+And Fe
3+Solution is measured a certain amount of test solution by ferritic composition, evenly mixes and is preheated to uniform temperature; Take by weighing a certain amount of oxalic acid ammonia by the coprecipitation reaction proportioning simultaneously and be made into certain density solution; Two kinds of solution are added in the 100ml aqueous solution simultaneously then, and stir 1h.Fully after the reaction, stop to stir, be cooled to room temperature.Precipitation is filtered, and the oxalates powder is made in washing after the drying.By the pH value of control charging rate and reaction system, the particle size of may command oxalates.This ferric oxalate is BaZnFe
6O
11The presoma of magnetic sintered body.
Secondly under carbon-dioxide protecting gas oxalates is put into quartz ampoule, keep taking out from electric furnace behind the 1h at 500 ℃, water quenching is prepared BaZnFe
6O
11Magnetic micro-powder.In this micro mist, add an amount of boride powder and make mixed-powder.
At last mixed-powder is filled in the mould, makes formed body after the pressurization.Keep 5 hours sintering to prepare sintered body in 900-1100 ℃ in carbon-dioxide protecting gas.This sintered body saturation magnetisation value is 40emu/g.Density is 5.2g/cm
2, Curie temperature is 90 degree ().
Embodiment 3
Make certain density Ba by preset blending ratio
2+, Fe
2+And Fe
3+Solution is measured a certain amount of test solution by ferritic composition, evenly mixes and is preheated to uniform temperature; Take by weighing a certain amount of oxalic acid ammonia by the coprecipitation reaction proportioning simultaneously and be made into certain density solution; Two kinds of solution are added in the 100ml aqueous solution simultaneously then, and stir 1h.Fully after the reaction, stop to stir, be cooled to room temperature.Precipitation is filtered, and yellow oxalates powder is made in washing after the drying.By the pH value of control charging rate and reaction system, the particle size of may command oxalates.This oxalates is the presoma of magnetic sintered body.
Secondly under carbon-dioxide protecting gas oxalates is put into quartz ampoule, keep taking out from electric furnace behind the 1h at 500 ℃, water quenching is prepared BaO6Fe
2O
3Magnetic micro-powder.In this micro mist, add an amount of boride powder and make mixed-powder.
At last mixed-powder is filled in the mould, makes formed body after the pressurization.Keep 5 hours sintering to prepare sintered body in 900-1100 ℃ in carbon-dioxide protecting gas.This sintered body saturation magnetisation value is 60emu/g.Density is 5.3g/cm
2, Curie temperature is 450 degree.
Embodiment 4
The preparation of low frequency MnZn, MnCuZn material
At first press the Mn of certain mol proportion
2+, Zn
2+, Cu
2+, Fe
3+Salting liquid evenly mix and be preheated to uniform temperature; Take by weighing a certain amount of oxalic acid ammonia by the coprecipitation reaction proportioning simultaneously and be made into certain density solution; Two kinds of solution are added in the 100ml aqueous solution simultaneously then, and stir 1h.Fully after the reaction, stop to stir, be cooled to room temperature.Precipitation is filtered, and presoma oxalates powder is made in washing after the drying.
Secondly under protection gas ferric oxalate is put into quartz ampoule, keep taking out from electric furnace behind the 1h at 500 ℃, water quenching is prepared magnetic MnZn, MnCuZn micro mist.In this micro mist, add an amount of additive and make mixed-powder.
At last mixed-powder is filled in the mould, pressurization 1MPa makes formed body.Low-temperature sintering is prepared MnZn, MnCuZn sintered body under protection gas.The high frequency magnetic permeability of this sintered body is 500, and high quality factor is 60, and three-point bending strength is 540MPa, is applicable to low frequency lamination inductance coil (referring to Fig. 6～8).
Embodiment 5
The preparation of medium-high frequency NiZn, NiCuZn material
At first press the Ni of certain mol proportion
2+, Zn
2+, Cu
2+, Fe
3+Salting liquid evenly mix and be preheated to uniform temperature; Take by weighing a certain amount of oxalic acid ammonia by the coprecipitation reaction proportioning simultaneously and be made into certain density solution; Simultaneously two kinds of solution are added in the 100ml aqueous solution then, and stir 1h.Fully after the reaction, stop to stir, be cooled to room temperature.Precipitation is filtered, and presoma mixing oxalates powder is made in washing after the drying.
Secondly under protection gas ferric oxalate is put into quartz ampoule, keep taking out from electric furnace behind the 1h at 500 ℃, water quenching is prepared magnetic NiZn, NiCuZn micro mist.In this micro mist, add an amount of additive and make mixed-powder.
At last mixed-powder is filled in the mould, the pressurization 1MPa, make formed body.Low-temperature sintering is prepared NiZn, NiCuZn sintered body under protection gas.This sintered body has high resistivity, and high quality factor and low-loss (as Fig. 9～Figure 10), are applicable to the lamination inductance coil that 20MHz is following.。
Embodiment 6
The very high frequency(VHF) preparation of Z type plane hexad ferrite material
At first press the Ba of certain mol proportion
2+, Co
2+, Fe
2+Salting liquid evenly mix and be preheated to uniform temperature; Take by weighing a certain amount of oxalic acid ammonia by the coprecipitation reaction proportioning simultaneously and be made into certain density solution; Two kinds of solution are added in the 100ml aqueous solution simultaneously then, and stir 1h.Fully after the reaction, stop to stir, be cooled to room temperature.Precipitation is filtered, and presoma oxalates powder is made in washing after the drying.
Secondly under protection gas ferric oxalate is put into quartz ampoule, keep taking out from electric furnace behind the 1h at 1000 ℃, water quenching is prepared high activity Z type plane hexad ferrite micro mist.In this micro mist, add an amount of additive and make mixed-powder.
At last mixed-powder is filled in the mould, the pressurization 1MPa, make formed body.Low-temperature sintering is prepared high activity Z type plane hexad ferrite sintered body under protection gas.This sintered body has high resistivity, and high quality factor and low-loss are applicable to very high frequency(VHF) lamination inductance coil.
Claims (11)
1. the manufacture method of a low-temperature sintering magnetic ferrites materials, this low-temperature sintering magnetic ferrites materials is used for inductance coil, it is characterized in that, this method comprises: utilize the mixed solution of one or more slaines and the solution of solubility oxalates to react, generate the operation 1 of the metal oxalate precipitation that is not soluted in water; The operation 2 that precipitation to operation 1 is filtered, washed; Product to operation 2 separates the operation 3 that back heating and decomposition under protection gas prepares the uniform ferrite micropowder of particle size distribution; In described micro mist, add composition and the content operation 4 that reach the effect of the sintering temperature of regulating sintered body and electromagnetic property of an amount of additive by regulating additive; With this powder is put into the mould extrusion forming, under protection gas, 800～1000 ℃ kept 1-20 hour down, sintering is made the operation 5 of sintered body.
2. the manufacture method of low-temperature sintering magnetic ferrites materials as claimed in claim 1 is characterized in that,
Described slaine is metal soluble salt classes such as iron, nickel, manganese, copper, zinc, barium, cobalt, strontium and magnesium.
3. the manufacture method of low-temperature sintering magnetic ferrites materials as claimed in claim 1 is characterized in that,
Described additive is calcic, silicon, bismuth or boron compound.
4. the manufacture method of low-temperature sintering magnetic ferrites materials as claimed in claim 1 is characterized in that,
Described protective atmosphere is a carbon dioxide.
5. the manufacture method of low-temperature sintering magnetic ferrites materials as claimed in claim 1 is characterized in that,
Can prepare the magnetic ferrites micro mist of different-grain diameter size by the control heat-treat condition, particle diameter is 0.1～10 μ m.
6. the manufacture method of low-temperature sintering magnetic ferrites materials as claimed in claim 1 is characterized in that,
Particle diameter is little to be greatly 5～30m of 0.1～1 μ m, specific area
2/ g.
7. the manufacture method of low-temperature sintering magnetic ferrites materials as claimed in claim 1 is characterized in that,
The average crystal grain diameter of described sintered body is 1～5 μ m.
8. the manufacture method of low-temperature sintering magnetic ferrites materials as claimed in claim 1 is characterized in that,
The density of described sintered body is 4～6g/cm
3
9. the manufacture method of low-temperature sintering magnetic ferrites materials as claimed in claim 1 is characterized in that,
The saturation magnetisation value of described sintered body is 30～90emu/g.
10. the manufacture method of low-temperature sintering magnetic ferrites materials as claimed in claim 1 is characterized in that,
The Curie temperature of described sintered body is 300～600 ℃.
11. the manufacture method of low-temperature sintering magnetic ferrites materials as claimed in claim 1 is characterized in that,
3 folding strengths of the machinery of described sintered body are 200～400MPa.
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|---|---|---|---|
| CN 200510135937 CN1812019A (en) | 2004-12-29 | 2005-12-29 | Low-temperature sintering production technology for magnetic ferrite and inductive material |
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| CN200410103636 | 2004-12-29 | ||
| CN200410103636.5 | 2004-12-29 | ||
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102217011A (en) * | 2008-08-13 | 2011-10-12 | 株式会社Emw | Method for producing ferrite |
| CN106431380A (en) * | 2016-09-05 | 2017-02-22 | 深圳顺络电子股份有限公司 | Method for preparing nano barium ferrite capable of being sintered under low temperature |
| CN113087516A (en) * | 2021-03-31 | 2021-07-09 | 重庆上甲电子股份有限公司 | Low-temperature sintering method for preparing manganese-zinc ferrite by using industrial wastes |
| TWI733320B (en) * | 2020-01-30 | 2021-07-11 | 奇力新電子股份有限公司 | Manufacturing method of multilayer inductance material capable of increasing saturation current and reducing magnetic loss |
| CN113257509A (en) * | 2020-02-07 | 2021-08-13 | 奇力新电子股份有限公司 | Method for manufacturing laminated inductance material capable of improving saturation current and reducing magnetic loss |
-
2005
- 2005-12-29 CN CN 200510135937 patent/CN1812019A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102217011A (en) * | 2008-08-13 | 2011-10-12 | 株式会社Emw | Method for producing ferrite |
| CN106431380A (en) * | 2016-09-05 | 2017-02-22 | 深圳顺络电子股份有限公司 | Method for preparing nano barium ferrite capable of being sintered under low temperature |
| TWI733320B (en) * | 2020-01-30 | 2021-07-11 | 奇力新電子股份有限公司 | Manufacturing method of multilayer inductance material capable of increasing saturation current and reducing magnetic loss |
| CN113257509A (en) * | 2020-02-07 | 2021-08-13 | 奇力新电子股份有限公司 | Method for manufacturing laminated inductance material capable of improving saturation current and reducing magnetic loss |
| CN113087516A (en) * | 2021-03-31 | 2021-07-09 | 重庆上甲电子股份有限公司 | Low-temperature sintering method for preparing manganese-zinc ferrite by using industrial wastes |
| CN113087516B (en) * | 2021-03-31 | 2022-07-22 | 重庆上甲电子股份有限公司 | Low-temperature sintering method for preparing manganese-zinc ferrite by using industrial wastes |
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Application publication date: 20060802 |