CN102557607A - Low-magnetism NiCu ferrite material and preparation method thereof - Google Patents
Low-magnetism NiCu ferrite material and preparation method thereof Download PDFInfo
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- CN102557607A CN102557607A CN2012100567696A CN201210056769A CN102557607A CN 102557607 A CN102557607 A CN 102557607A CN 2012100567696 A CN2012100567696 A CN 2012100567696A CN 201210056769 A CN201210056769 A CN 201210056769A CN 102557607 A CN102557607 A CN 102557607A
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Abstract
The invention discloses a low-magnetism NiCu ferrite material and a preparation method thereof. An electronic part is manufactured by the low-magnetism NiCu ferrite material, so the electronic part is more reliable. According to the low-magnetism NiCu ferrite material, the main components comprise 86 to 94 molar percent of NiO, 5 to 9 molar percent of CuO and the balance of Fe2O3; a sintering aid is 5 to 9 percent of the weight of the main components; an additive Co2O3 is 1 to 3 percent of the weight of the main components; an additive CuO is 0.5 to 1.5 percent of the weight of the main components; and an additive beta-eucryptite is 0.5 to 1.5 percent of the weight of the main components. The invention also provides the preparation method of the low-magnetism NiCu ferrite material. When the frequency is 1 MHz, the initial magnetic conductivity of the material is 1.4 to 1.6; the microstructure is similar to the main ferrite material; the thermal expansion coefficient can be improved in wide temperature range; and the problem of unreliability of the electronic parts is solved.
Description
Technical field
The present invention relates to Ferrite Material and preparation method thereof, particularly relate to a kind of low magnetic NiCu Ferrite Material that is applied to coil part and preparation method thereof.
Background technology
In recent years lamination power inductance product usage quantity in power circuit increasing, require increasingly highly, we are in order further to improve the overlapping performance of direct current that the power supply service efficiency need improve lamination power inductance product.Mainly improve raising at present from two aspects: one of which improve Ferrite Material the overlapping performance of direct current, another introduces the air gap interlayer in product design.
For the air gap interlayer, mainly contain at present and use stupalith and low magnetic ferrites material.Chinese patent CN1241870 Granted publication a kind of nonmagnetic ceramic and laminated ceramic parts; Said nonmagnetic ceramic contains the borosilicate glass of 35-75 (weight) % as matrix; And disperse has the alpha-quartz of 5-40 (weight) % and the zinc silicate of 5-60 (weight) %, the SiO of said borosilicate glass in the substrate
2And B
2O
3Content is respectively 70-90 (weight) % and 10-30 (weight) %.Adopt said nonmagnetic ceramic can make the multilayer ceramic inductance, have the premium properties of low-k and good aspects such as high frequency characteristics.But in some cases, kinds of materials often demonstrates different separately thermal expansivity, and difference is very big each other, especially between Ferrite Material and the stupalith.Therefore; Because the difference of thermal expansion and contraction between the various materials of multilayer body that sintering causes; Make the inner thermal stresses that produces of lamination sintered compact in the process of cooling after sintering; Thereby make the distortion of lamination sintered compact or produce outside, internal fissure, can have influence on the safety of compounded multilayer electronic component.If form similar low magnetic ferrites material with inducer, just can avoid the sintering matching problem of out-phase material.
In addition, Chinese patent CN101017728A discloses a kind of nonmagnetic Zn ferrite and the compounded multilayer electronic component that uses it, said a kind of nonmagnetic Zn ferrite, and it is characterized in that: red stone is with Fe
2O
3Conversion contains 45-49.7 mole (mol) %, and surplus is made up of zinc oxide (ZnO conversion), wherein Fe
2+Amount be 1 (weight) below the %, do not contain Cu and high resistivity arranged.High resistivity can be provided and not contain Cu and the low magnetic NiZn Ferrite Material and the material manufacturing method thereof that obtain.But this patent mainly is in order to obtain high-resistance low magnetic ferrites material, does not relate to solution that two phase materials burn relevant thermal expansivity altogether and does not also relate to various sintering agents and the additive among this paper simultaneously.
Therefore; Ferrite Material of the prior art; Do not relate to a kind ofly both had low magnetic, microstructure is similar with main material Ferrite Material; The thermal expansivity of wide temperature range can be provided again, burn difference because of thermal expansivity altogether and cause the sintered compact distortion or produce outside, internal fissure problem causing the insecure Ferrite Material of electronic unit to solve two phase Ferrite Materials.
Summary of the invention
The technical problem that the present invention will solve is the defective that remedies above-mentioned prior art, provides a kind of electronic unit that makes more reliable, is applied to the low magnetic NiCu Ferrite Material in this electronic unit.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of low magnetic NiCu Ferrite Material, and main composition is pressed the NiO of mol per-cent by 86-94mol%, the CuO of 5-9mol%, surplus is Fe
2O
3Form; Also add the sintering agent of becoming owner of composition weight 5-9wt% and by the addition of C o of main composition weight percent meter
2O
31-3wt%, CuO 0.5-1.5wt%, beta-eucryptite 0.5-1.5wt%.
Sintering agent according to the invention is Bi
2O
3, ZnO, B
2O
3In more than one.
NiO in the main composition according to the invention is preferably 88-91.8mol%.
CuO in the main composition according to the invention is preferably 7mol%.
Sintering agent according to the invention is preferably 7wt%.
Co in the additive according to the invention
2O
3Be preferably 2wt%.
CuO in the additive according to the invention is preferably 1wt%.
Beta-eucryptite in the additive according to the invention is preferably 1wt%.
A kind of preparation method of low magnetic NiCu Ferrite Material may further comprise the steps: one, press mol per-cent metering, taking by weighing NiO 86-94mol%, CuO 5-9mol%, surplus is Fe
2O
3, the pure water of weight such as adding is with ball mill batch mixing 24 hours, slurry; Two, slurry is placed 150 ℃ of baking oven oven dry 48 hours, get powder; Three, powder is crossed 40 order moto-vibro screens, temperature 850-950 ℃ of following pre-burning 2 hours, after naturally cool to room temperature; Four, adding is by the sintering agent 5-9wt% and the addition of C o of the material weight per-cent after the pre-burning
2O
31-3wt%, CuO 0.5-1.5wt%, beta-eucryptite 0.5-1.5wt% must mix the back material; Sintering agent is Bi
2O
3, ZnO, B
2O
3In more than one; Five, add once more with the pure water that mixes weight such as back material and use levigate the processing to median size of ball mill batch mixing to be 0.8-1.2 μ m; Six, the slurry behind the ball milling is placed 150 ℃ of baking oven oven dry 48 hours; Seven, the powder after will drying is crossed 40 order moto-vibro screens; Eight, add the polyvinyl alcohol water solution of powder 10% weight, this polyvinyl alcohol water solution concentration is 10%, in agate mortar, mixes 30min, crosses 40 eye mesh screens; Nine, according to 3.1g/cm
3Compact density, adopt the shape that prior art is pressed into to be needed; Ten, under 900 ℃ in sinter machine sintering 2 hours, be made into low magnetic NiCu Ferrite Material.
The said sintering agent of preparation method of the low magnetic NiCu Ferrite Material of the present invention and additive are preferably in the levigate treating processes after pre-burning or adding afterwards.
Low magnetic NiCu Ferrite Material sintered density provided by the invention is at 6.00g/cm
3More than, the initial permeability μ i under the 1MHz is between 1.4～1.6; In the compositing range of above-mentioned main composition, when NiO is lower than 86mol%, be difficult to make the material initial permeability to be low to moderate 1.4-1.6, and NiO is when being higher than 94mol%, microstructure aspect and main material Ferrite Material difference are bigger.When CuO was lower than 5mol%, the material sintering activity was relatively poor, caused sintering to produce internal stress; And CuO also is difficult to make the material initial permeability to be low to moderate 1.4-1.6 when being higher than 9mol%.In addition, in the compositing range with respect to the secondary composition of above-mentioned main composition, if the content of sintering agent is lower than 5wt%, the material sintering character reduces; And the content of sintering agent is higher than 9wt%, thereby then causes material grains to be grown up unusually easily and main body Ferrite Material microstructure differs bigger.If Co in the additive
2O
3Content be lower than 1wt%, the material initial permeability is difficult to be low to moderate 1.4～1.6, material thermal expansion coefficient and shrinking percentage are difficult in wide temperature range, adjust; And Co
2O
3Content be higher than 3wt%, same material thermal expansion coefficient and shrinking percentage are difficult in wide temperature range, adjust.If the content of beta-eucryptite is lower than 0.5wt% in the additive, material thermal expansion coefficient and shrinking percentage are difficult in wide temperature range, adjust; And the content of beta-eucryptite is higher than 1.5wt%, and relatively poor, low magnetic NiCu Ferrite Material microstructure of material sintering activity and main body Ferrite Material differ bigger.If the content of CuO is lower than 0.5wt% in the additive, material thermal expansion coefficient and shrinking percentage are difficult in wide temperature range, adjust; And the content of CuO is higher than 1.5wt%, tends to then that material causes that crystal grain is grown up unusually, material thermal expansion coefficient and shrinking percentage be difficult in wide temperature range, adjust.
The correlated beneficial effect of the present invention and prior art is; The initial permeability of material of the present invention when frequency is 1MHz is low to moderate the similar of its average grain size and main material Ferrite Material aspect 1.4-1.6, the microstructure, specifically can in awide temperature range, improve the thermal expansivity of Ferrite Material.Can effectively solve the two-phase Ferrite Material burns difference because of thermal coefficient of expansion altogether and causes the sintered body distortion or produce outside, underbead crack making the insecure problem of electronic unit.
Embodiment
The present invention will be described in more detail through enumerating concrete embodiment below.Low magnetic NiCu Ferrite Material of the present invention is a kind of with Ni ion, Cu ion, the Fe ion low magnetic ferrites materials of synthetic spinel type at high temperature.Sintered density (the g/cm of the Ferrite Material that in following examples, prepares
3) high more explanation adopts the unfailing performance of electron device of Ferrite Material of the present invention good more; Electron device under the same thickness situation, the low more explanation of initial permeability μ i under its 1MHz, the electric property of this electron device is good more; With the thermal expansivity (10 of Ferrite Material of the present invention at 100～800 ℃
-6M/ ℃) to compare with the ferritic thermal expansivity of main material, its value is approximate with the thermal expansivity of main material Ferrite Material, the problem that causes the sintered compact distortion or crack with the common burning that solves two phase materials; Compare with the ferritic final shrinking percentage value of main material with Ferrite Material of the present invention final shrinking percentage value behind 900 ℃ of sintering; Its value is approximate with the final shrinking percentage value of main material Ferrite Material, the problem that causes the sintered compact distortion or crack with the common burning that solves two phase materials.
Embodiment 1
One, presses the metering of mol per-cent, take by weighing NiO 91.8mol%, CuO 7.0mol%, Fe
2O
31.2mol%, the pure water of weight such as adding obtains slurry with ball mill batch mixing 24 hours;
Two, slurry is placed 150 ℃ of baking oven oven dry 48 hours, obtain powder;
Three, powder is crossed 40 order moto-vibro screens after, 900 ℃ of box type sintering ovens of temperature pre-burning 2 hours, after naturally cool to room temperature;
Four, add in the material after pre-burning, by the sintering agent Bi of material weight per-cent
2O
32wt%, B
2O
32wt%, ZnO 1wt% and addition of C o
2O
31.0wt%, CuO 0.5wt%, beta-eucryptite 0.5wt%;
Five, the pure water of weight such as adding uses levigate the processing to median size of ball mill batch mixing to be to obtain slurry by 0.8-1.2 μ m once more;
Six, slurry is placed 150 ℃ of baking oven oven dry 48 hours, obtain powder;
Seven, powder is crossed 40 order moto-vibro screens;
Eight, add the polyvinyl alcohol water solution of powder 10% weight, this polyvinyl alcohol water solution concentration is 10%, in agate mortar, mixes 30min, crosses 40 eye mesh screens;
Nine, according to 3.1g/cm
3Compact density, adopt prior art to be pressed into external diameter 42mm, internal diameter 30mm, highly to be the disk of the magnet ring of 3.5mm and Φ 12mm * H2mm;
Ten, under 900 ℃ in sinter machine sintering 2 hours, be made into the magnet ring shape sample and the disc sample of low magnetic NiCu Ferrite Material.
Embodiment 2
Concrete steps are with embodiment 1, but beta-eucryptite is 1.5wt% in step 4.
Embodiment 3
Concrete steps are with embodiment 1, but in step 4 sintering agent Bi
2O
3Be 4wt%, B
2O
3For 2wt%, ZnO are 1wt%, CuO is 1.5wt% in the additive.
Embodiment 4
Concrete steps are with embodiment 1, but NiO is that 88.0mol%, CuO are 9.0mol%, Fe in step 1
2O
3Be 3.0mol%.Calcined temperature is 950 ℃ in the step 3.Addition of C o in the step 4
2O
3For 3.0wt%, CuO are that 1.5wt%, beta-eucryptite are 1.5wt%.
Embodiment 5
Concrete steps are with embodiment 1, but NiO is that 88.0mol%, CuO are 9.0mol%, Fe in step 1
2O
3Be 3.0mol%.Calcined temperature is 950 ℃ in the step 3.Sintering agent Bi in the step 4
2O
3Be 4wt%, B
2O
3For 2wt%, ZnO are 1wt%, Co in the additive
2O
3Be 3.0wt%.
Embodiment 6
Concrete steps are with embodiment 1, but NiO is that 88.0mol%, CuO are 9.0mol%, Fe in step 1
2O
3Be 3.0mol%.Calcined temperature is 950 ℃ in the step 3.Sintering agent Bi in the step 4
2O
3Be 4wt%, B
2O
3For 2wt%, ZnO are 1wt%, addition of C o
2O
3For 3.0wt%, beta-eucryptite are 1.5wt%.
Embodiment 7
Concrete steps are with embodiment 1, but NiO is that 86.0mol%, CuO are 5.0mol%, Fe in step 1
2O
3Be 9.0mol%.Calcined temperature is 850 ℃ in the step 3.Sintering agent Bi in the step 4
2O
3Be 6wt%, B
2O
3For 2wt%, ZnO are 1wt%.
Embodiment 8
Concrete steps are with embodiment 1, but NiO is that 86.0mol%, CuO are 5.0mol%, Fe in step 1
2O
3Be 9.0mol%.Calcined temperature is 850 ℃ in the step 3.Sintering agent Bi in the step 4
2O
3Be 4wt%, B
2O
3Be 2wt%, ZnO 1wt%, addition of C o
2O
3For 3.0wt%, beta-eucryptite are 1.5wt%.
Embodiment 9
Concrete steps are with embodiment 1, but NiO is that 94.0mol%, CuO are 5.0mol%, Fe in step 1
2O
3Be 1.0mol%.Calcined temperature is 850 ℃ in the step 3.Sintering agent Bi in the step 4
2O
3Be 4wt%, B
2O
3Be 2wt%, ZnO 1wt%, addition of C o
2O
3Be 3.0wt%.
Embodiment 10
Concrete steps are with embodiment 1, but NiO is that 94.0mol%, CuO are 5.0mol%, Fe in step 1
2O
3Be 1.0mol%.Calcined temperature is 850 ℃ in the step 3.Sintering agent Bi in the step 4
2O
3Be 4wt%, B
2O
3For 2wt%, ZnO are 1wt%, addition of C o
2O
3For 2.0wt%, CuO are that 1.0wt%, beta-eucryptite are 1.0wt%.
The magnet ring shape sample and the disc sample of the low magnetic NiCu Ferrite Material of processing to above embodiment are measured following data: the density of (1) sintered compact; (2) the initial permeability μ i under the 1MHz; (3) 100～800 ℃ cte value; (4) final shrinking percentage value.
The testing method of above-mentioned (1)～(4) association is following:
(1) density of sintered compact
With the test of Archimedes's method, utilize the numerical evaluation that records to draw the density p (g/cm of unit of low magnetic NiCu Ferrite Material
3).
(2) the initial permeability μ i under the 1MHz
Behind the surface of magnet ring shape sample and disc sample difference uniform winding 20 circle insulated copper wires, with Agilent (U.S.'s Agilent science and technology) the inductance value Ls of equipment E4991+16192 test fixture test under 1MHz, through formula (Ls=μ
0μ
γN
2S/l) conversion draws low magnetic NiCu Ferrite Material initial permeability μ i.
(3) cte value
Use the elevated temperature heat coefficient of expansion tester (model DIL402PC) of the anti-company of speeding of Germany; The low thermal expansion curve of magnetic NiCu Ferrite Material under 25～900 ℃ of test draws at 100～800 ℃ of following material coefficient of thermal expansion coefficients through software NETZSCH Proteus Thermal Analysis (the hot analysis software of the anti-Proteus of speeding) analysis.
(4) final shrinking percentage value
The outside dimension L of each embodiment magnet ring shape sample and disc sample behind the test sintering calculates low magnetic NiCu Ferrite Material final shrinking percentage value behind 900 ℃ of sintering through formula (42-L)/42*100%.
Its result is as shown in table 1.
Table 1
Can know that from last table result effect of the present invention is tangible; Low magnetic NiCu Ferrite Material according to the invention is when having low magnetic, microstructure and main material Ferrite Material is similar; The thermal expansivity of wide temperature range can be provided especially, improve the common burning behavior of low magnetic ferrites material and main material Ferrite Material.
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.Those of ordinary skill for technical field under the present invention; Under the prerequisite that does not break away from the present invention's design, make some alternative or obvious modification that are equal to; And performance or purposes are identical, all should be regarded as belonging to the scope of patent protection that the present invention is confirmed by claims of being submitted to.
Claims (10)
1. one kind low magnetic NiCu Ferrite Material, it is characterized in that: main composition is pressed the NiO of mol per-cent by 86-94mol%, the CuO of 5-9mol%, surplus is Fe
2O
3Form; Also add the sintering agent of becoming owner of composition weight 5-9wt% and by the addition of C o of main composition weight percent meter
2O
31-3wt%, CuO 0.5-1.5wt%, beta-eucryptite 0.5-1.5wt%.
2. low magnetic NiCu Ferrite Material according to claim 1, it is characterized in that: said sintering agent is Bi
2O
3, ZnO, B
2O
3In more than one.
3. low magnetic NiCu Ferrite Material according to claim 1 and 2 is characterized in that: the NiO in the said main composition is 88-91.8mol%.
4. low magnetic NiCu Ferrite Material according to claim 3 is characterized in that: the CuO in the said main composition is 7mol%.
5. low magnetic NiCu Ferrite Material according to claim 4 is characterized in that: said sintering agent is 7wt%.
6. low magnetic NiCu Ferrite Material according to claim 5 is characterized in that: the Co in the said additive
2O
3Be 2wt%.
7. low magnetic NiCu Ferrite Material according to claim 6 is characterized in that: the CuO in the said additive is 1wt%.
8. low magnetic NiCu Ferrite Material according to claim 2 is characterized in that: the beta-eucryptite in the said additive is 1wt%.
9. the preparation method of a low magnetic NiCu Ferrite Material may further comprise the steps:
One, press mol per-cent metering, taking by weighing NiO 86-94mol%, CuO 5-9mol%, surplus is Fe
2O
3, the pure water of weight such as adding is with ball mill batch mixing 24 hours, slurry;
Two, slurry is placed 150 ℃ of baking oven oven dry 48 hours, get powder;
Three, powder is crossed 40 order moto-vibro screens, temperature 850-950 ℃ of following pre-burning 2 hours, after naturally cool to room temperature;
Four, adding is by the sintering agent 5-9wt% and the addition of C o of the material weight per-cent after the pre-burning
2O
31-3wt%, CuO 0.5-1.5wt%, beta-eucryptite 0.5-1.5wt% must mix the back material; Sintering agent is Bi
2O
3, ZnO, B
2O
3In more than one;
Five, add once more with the pure water that mixes weight such as back material and use levigate the processing to median size of ball mill batch mixing to be 0.8-1.2 μ m;
Six, the slurry behind the ball milling is placed 150 ℃ of baking oven oven dry 48 hours;
Seven, the powder after will drying is crossed 40 order moto-vibro screens;
Eight, add the polyvinyl alcohol water solution of powder 10% weight, this polyvinyl alcohol water solution concentration is 10%, in agate mortar, mixes 30min, crosses 40 eye mesh screens;
Nine, according to 3.1g/cm
3Compact density, adopt the shape that prior art is pressed into to be needed;
Ten, under 900 ℃ in sinter machine sintering 2 hours, be made into low magnetic NiCu Ferrite Material.
10. a kind of method for preparing low magnetic NiCu Ferrite Material according to claim 9 is characterized in that: add in said sintering agent and the additive levigate treating processes after pre-burning or afterwards.
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|---|---|---|---|---|
| CN103626515A (en) * | 2013-12-02 | 2014-03-12 | 深圳顺络电子股份有限公司 | Laminated component and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102122557A (en) * | 2010-12-14 | 2011-07-13 | 深圳顺络电子股份有限公司 | Low magnetic ferrite material and manufacturing method thereof |
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|---|---|---|---|---|
| CN102122557A (en) * | 2010-12-14 | 2011-07-13 | 深圳顺络电子股份有限公司 | Low magnetic ferrite material and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626515A (en) * | 2013-12-02 | 2014-03-12 | 深圳顺络电子股份有限公司 | Laminated component and production method thereof |
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Application publication date: 20120711 |