CN103714931B - A kind of ferrite powder and preparation method thereof - Google Patents
A kind of ferrite powder and preparation method thereof Download PDFInfo
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- CN103714931B CN103714931B CN201310643115.8A CN201310643115A CN103714931B CN 103714931 B CN103714931 B CN 103714931B CN 201310643115 A CN201310643115 A CN 201310643115A CN 103714931 B CN103714931 B CN 103714931B
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Abstract
The invention discloses a kind of ferrite powder and preparation method thereof, this ferrite powder includes ferrite particle and silicon dioxide layer, and the particle diameter of ferrite particle is 0.5～2.0 μm, and the surface of each ferrite particle is all coated with silicon oxide layer.Preparation method includes: (1) prepares the ferrite particle I that particle diameter is 0.5～2.0 μm；(2) cleaning ferrite particle I with the HCl of 0.5～2mol/L and filter, filter cake cleans and dries the ferrite particle II obtaining being dried；(3) ferrite particle II is added in alcohols solvent, it is sufficiently stirred for dispersion after adding dispersant, adds ammonia and stir, then be added dropwise over tetraethyl orthosilicate, tetraethyl orthosilicate generates silicon dioxide, makes the outer surface of each ferrite particle II all be coated with silicon oxide.The present invention reduces Ferrite Material curtain coating tablet perforate dust by improving ferrite powder, fundamentally solves the dust residue problem after tablet punching, and does not affect the effective of interior electrode and through hole junction point and be connected.
Description
Technical field
The present invention relates to magnetic material, particularly relate to a kind of ferrite powder and preparation method thereof.
Background technology
In recent years, along with the extensive application of electronic devices and components, while focusing on components and parts performance, the most more pay close attention to
The reliability of components and parts.When dry process platform makes the most common laminated sheet type electronic component, need
Laser boring on base material tablet, forms a through hole, to ensure that electrode is connected with the effective of last layer electrode.Ferrum
Tablet laser boring after ferrite slurrying curtain coating, understands residual dust around through-hole aperture and in hole, difference is joined
After the ferrite curtain coating tablet punching of side, dust residual condition can be variant.On tablet, electrode system is carried out after punching
When making, the Ferrite dust around through hole and in hole can be mixed in electrode slurry, when dust residual is more, and can shadow
Ring electrode conduction effect, cause product to have open circuit risk；A small amount of dust is mixed in electrode slurry, also can increase
The D.C. resistance of electrode, affects the Performance And Reliability of components and parts.
In the scheme of existing reduction dust, mainly there are two kinds of measures, after one is to increase the punching of ferrite tablet
Dust-removing process.But this technology has open defect: 1, require strictly for cleaner, part ferrite
After formula curtain coating tablet perforate, around through hole, web surface dust accumulation is serious, if dedusting bristle stiffness is not enough,
Around through hole, dust is difficult to be swept；If dedusting bristle stiffness is too hard, can scratch curtain coating web surface.Both of which
Electrode, the turn-on effect of through hole connection can be affected；If 2 cleaning brush are when clearing up the dust of web surface,
Dust fails the most thoroughly to discharge, and dust can be gathered in inside through hole, affects the turn-on effect that through hole connects, deposits
In open circuit risk.Two is to use solid-state laser hole making drill replacement common laser tapping machine, but this kind of measure employing
Equipment cost is higher.
Summary of the invention
The technical problem to be solved is: make up above-mentioned the deficiencies in the prior art, proposes a kind of ferrite
Powder body and preparation method thereof, reduces Ferrite Material curtain coating tablet perforate dust by improving ferrite powder,
Fundamentally solve the dust residue problem after tablet punching, and do not affect having of interior electrode and through hole junction point
Effect connects.
The technical problem of the present invention is solved by following technical scheme:
A kind of ferrite powder, the particle diameter of described ferrite particle is 0.5～2.0 μm, also includes silicon dioxide layer,
The surface of each described ferrite particle is all coated with described silicon dioxide layer.
Preferably, the particle diameter of described ferrite particle is 0.8～1.2 μm.
The preparation method of a kind of above-mentioned ferrite powder, comprises the steps:
(1) ferrite particle I that particle diameter is 0.5～2.0 μm is prepared；
(2) clean described ferrite particle I with the HCl solution of 0.5～2mol/L and filter to remove described ferrum
Being dissolved in the foreign ion of described HCl solution in oxysome microgranule I, filter cake cleans and dries the ferrum oxygen obtaining being dried
Body microgranule II；
(3) described ferrite particle II is added in alcohols solvent, after adding dispersant, is sufficiently stirred for dispersion,
It is subsequently adding after ammonia stirs, then is added dropwise over tetraethyl orthosilicate, by the hydrolysis of described tetraethyl orthosilicate
Silicon dioxide is generated so that the outer surface of each ferrite particle II is all coated with described dioxy with condensation reaction
SiClx.
Preferably, the particle diameter of ferrite particle I described in step (1) is 0.8～1.2 μm.
Preferably, ammonia described in step (3) accounts for the 5～10% of described ferrite particle II mass, described just
Silester accounts for the 1～10% of described ferrite particle II mass.
Preferably, described ammonia accounts for the 5～7% of described ferrite particle II mass.
Preferably, described tetraethyl orthosilicate accounts for the 3～5% of described ferrite particle II mass.
Preferably, in step (2), by molten for the HCl that described ferrite particle I is immersed in 0.8～1.0mol/L
In liquid, it is sufficiently stirred for 2～5 hours, after filtration, filter cake deionized water and dehydrated alcohol is alternately cleaned 1～5
Secondary.
Preferably, described dispersant accounts for the 1～5% of described ferrite particle II mass.
Preferably, comprise the steps:
(1) Ferrite Material uses ball milling prepare ferrite particle I that particle diameter is 0.8～1.2 μm；
(2) described ferrite particle I is immersed in the HCl solution of 0.8～1mol/L, is sufficiently stirred for 2～5
Hour, then filter, filter cake deionized water and dehydrated alcohol are alternately cleaned 3～4 post-dryings and is dried
Ferrite particle II；；
(3) described ferrite particle II is joined in ethanol, and addition accounts for described ferrite particle II mass
2～3% dispersant after be sufficiently stirred for dispersion, add and account for the 5～7% of described ferrite particle II mass
After ammonia stirs, then it is added dropwise over accounting for 3～the tetraethyl orthosilicate of 5% of described ferrite particle II mass,
Hydrolysis and condensation reaction by described tetraethyl orthosilicate generate silicon dioxide so that each ferrite particle II
Outer surface be all coated with described silicon dioxide.
The present invention is compared with the prior art and provides the benefit that: the tablet being cast out with the ferrite powder of the present invention
Perforate dust can be greatly lowered, improve near through hole and internal dust, and do not affect interior electrode with
Effective connection of through hole junction point, can reduce product open circuit risk, improve the reliability of components and parts.
Accompanying drawing explanation
Fig. 1 is the microscopic appearance figure of the tablet obtained in the embodiment of the present invention one；
Fig. 2 is the picture after the tablet punching obtained in the embodiment of the present invention one；
Fig. 3 is the microscopic appearance figure of the tablet obtained in comparative example of the present invention；
Fig. 4 is the picture after the tablet punching obtained in comparative example of the present invention.
Detailed description of the invention
Below against accompanying drawing and combine preferred embodiment the invention will be further described.
The present invention provides a kind of ferrite powder, in one embodiment, including ferrite particle and silicon dioxide
Layer, the particle diameter of described ferrite particle is 0.5～2.0 μm, and the surface of each described ferrite particle is all coated with
Described silicon dioxide layer.
In a preferred embodiment, the particle diameter of ferrite particle is 0.8～1.2 μm.
The present invention also provides for the preparation method of a kind of ferrite powder, in one embodiment, including walking as follows
Rapid:
(1) ferrite particle I that particle diameter is 0.5～2.0 μm is prepared；
(2) clean described ferrite particle I with the HCl solution of 0.5～2mol/L and filter to remove described ferrum
Being dissolved in the foreign ion of described HCl solution in oxysome microgranule I, filter cake cleans and dries the ferrum oxygen obtaining being dried
Body microgranule II；
(3) described ferrite particle II is added in alcohols solvent, after adding dispersant, is sufficiently stirred for dispersion,
It is subsequently adding after ammonia stirs, then is added dropwise over tetraethyl orthosilicate, by the hydrolysis of described tetraethyl orthosilicate
Silicon dioxide is generated so that the outer surface of each ferrite particle II is all coated with described dioxy with condensation reaction
SiClx.
In some other preferred embodiment: described in step (1), the particle diameter of ferrite particle I is
0.8～1.2 μm.It is 5～10%(the most excellent that ammonia described in step (3) accounts for described ferrite particle II mass
Elect 5～7% as) described tetraethyl orthosilicate accounts for the 1～10%(of described ferrite particle II mass more preferably
3～5%).In step (2), described ferrite particle I is immersed in the HCl solution of 0.8～1.0mol/L,
It is sufficiently stirred for 2～5 hours, after filtration, filter cake deionized water and dehydrated alcohol is alternately cleaned 1～5 time.Described
Dispersant accounts for the 1～5%(of described ferrite particle II mass more preferably 2～3%).Alcohols solvent is permissible
Be first, second, third, butanol etc., the consumption of alcohols solvent be enough to make ferrite particle I disperse wherein and ferrite
Microgranule I will not be reunited.
Below by way of more specifically embodiment and a corresponding comparative example, the present invention is further elaborated.
Embodiment one
Using NiZnCu Ferrite Material, ferrite particle and mol percentage ratio thereof include the following:
Fe2O3: 46mol%；
ZnO:27mol%；
CuO:9mol%；
NiO:18mol%；
Being made ferrite powder by above-mentioned ferrite particle, step includes:
(1) each composition of above-mentioned mol percentage ratio is mixed, then with etc. the pure water of weight grind with ball mill batch mixing
Carefully process to the slurry that mean diameter is 0.8～1.5 μm, slurry be placed in 150 DEG C of baking ovens baking 48 hours,
Cross 40 mesh sieves after drying and obtain required ferrite particle I.
(2) HCl solution of ferrite particle 1.0mol/L is soaked, be sufficiently stirred for 2 hours, then mistake
Filter separates, and is intersected with appropriate deionized water and dehydrated alcohol by filter cake and cleans what 3 post-dryings obtained being dried
Ferrite particle II.
(3) ferrite particle II is added in ethanol, and add the basis accounting for ferrite particle II mass 3wt%
It is sufficiently stirred for dispersion after the dispersant that field is conventional, then addition accounts for ferrite particle II mass in mixture
The ammonia of 5wt% stirs, is more under agitation added dropwise over accounting for the positive silicic acid of ferrite particle II mass 5wt%
Ethyl ester, mix and blend, after 12 hours, is filtrated to get ferrite powder, at each ferrum in this ferrite powder
The outer surface of oxysome microgranule II is all coated with silicon oxide layer, and it is standby to clean 5 post-dryings with pure water.By upper
State that the ferrite powder that obtains makes curtain coating tablet, the step of punching includes:
(1) in ferrite powder, addition accounts for the volume ratio of ferrite powder weight 40wt% is 1:1 acetic acid third
Ester, with the solvent of isobutanol, is subsequently added into the poly-methyl-prop of organic bond accounting for ferrite powder weight 70wt%
E pioic acid methyl ester (PMMA) and account for the dispersant Triton X-100 of ferrite powder weight 1.2wt%
(X-100) and account for the plasticizer phthalic acid dibutyl ester of ferrite powder weight 2.6wt%, ball mill is used to stir
Mix, form ferrite slurry after continuing 16 hours with the rotating speed of 45r/min, be then cast by casting technique
The tablet of 15 μ m-thick, is cut off by 152.4mm*152.4mm size, forms ferrite substrate.
(2) ferrite substrate (hereinafter referred to as tablet) is punched with laser machine.
Tablet after above-mentioned punching is tested as follows:
(1) sampling: center arda sampling on tablet after drilling.
(2) outward appearance: use Tescan VEGA3EPH scanning electron microscope and energy disperse spectroscopy integral machine to carry out image
Gathering and component analysis, result is: it is 0.81% that composition Si accounts for the mass fraction of ferrite substrate quality；Material
The microscopic appearance of sheet as it is shown in figure 1, the picture after tablet punching as shown in Figure 2.
Comparative example
Difference with embodiment one is: the ferrite particle under embodiment one formula directly makes curtain coating material
Sheet, punching, step is as follows:
(1) each composition of above-mentioned mol percentage ratio is mixed, then with etc. the pure water of weight grind with ball mill batch mixing
Carefully process to the slurry that mean diameter is 0.8～1.5 μm, slurry be placed in 150 DEG C of baking ovens baking 48 hours,
Cross 40 mesh sieves after drying and obtain required ferrite particle.
2) in ferrite particle, addition accounts for the volume ratio of ferrite particle quality 40wt% is 1:1 propyl acetate
With the solvent of isobutanol, it is subsequently added into the organic bond polymethylacrylic acid accounting for ferrite particle quality 70wt%
Methyl ester (PMMA) and account for the dispersant Triton X-100 (X-100) of ferrite particle quality 1.2wt%
With account for the plasticizer phthalic acid dibutyl ester of ferrite particle quality 2.6wt%, use ball mill stirring, with
The rotating speed of 45r/min forms ferrite slurry after continuing 16 hours, is then cast 15 μ m-thick by casting technique
Tablet, by 152.4mm*152.4mm size cut off, formed ferrite substrate.
3) ferrite substrate (hereinafter referred to as tablet) is punched with laser machine.
Tablet after above-mentioned punching is carried out the test of same embodiment one, the microscopic appearance of tablet as it is shown on figure 3,
Picture after tablet punching is as shown in Figure 4.
The result recorded from embodiment one, uses said method preferably can be coated with on ferrite particle surface
Upper SiO2.From embodiment one and the comparing result of comparative example: at ferrite particle outer cladding silicon dioxide
Afterwards tablet perforate dust is had clear improvement, such that it is able to reduce product open circuit risk, improve the reliable of components and parts
Property.
In addition to the NiZnCu Ferrite Material in above example, other Ferrite Materials can also be with this
Bright method processes, such as: Mn-Zn, Cu-Zn Ferrite Material etc..
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to
Assert the present invention be embodied as be confined to these explanations.For those skilled in the art
For, without departing from the inventive concept of the premise, it is also possible to make some equivalents and substitute or obvious modification, and
And performance or purposes identical, all should be considered as belonging to protection scope of the present invention.
Claims (1)
1. the preparation method of a ferrite substrate, it is characterised in that comprise the steps:
(1) Ferrite Material uses ball milling prepare ferrite particle I that particle diameter is 0.8～1.2 μm；
(2) described ferrite particle I is immersed in the HCl solution of 0.8～1mol/L, is sufficiently stirred for 2～5
Hour, then filter, filter cake deionized water and dehydrated alcohol are alternately cleaned 3～4 post-dryings and is dried
Ferrite particle II；
(3) described ferrite particle II is joined in ethanol, and addition accounts for described ferrite particle II mass
2～3% dispersant after be sufficiently stirred for dispersion, add and account for the 5～7% of described ferrite particle II mass
After ammonia stirs, then it is added dropwise over accounting for 3～the tetraethyl orthosilicate of 5% of described ferrite particle II mass,
Obtaining ferrite powder, hydrolysis and condensation reaction by described tetraethyl orthosilicate generate silicon dioxide so that every
The outer surface of one ferrite particle II is all coated with described silicon dioxide；
(4) in described ferrite powder, addition accounts for the volume ratio of ferrite powder weight 40wt% is 1:1 vinegar
Propyl propionate, with the solvent of isobutanol, is subsequently added into the poly-first of organic bond accounting for ferrite powder weight 70wt%
Base acrylic acid methyl ester. and account for the dispersant Triton X-100 of ferrite powder weight 1.2wt% and account for ferrum
The plasticizer phthalic acid dibutyl ester of oxysome powder quality 2.6wt%, uses ball mill stirring, with 45r/min
Rotating speed continue to be formed after 16 hours ferrite slurry, be then cast by casting technique, formation ferrite base
Sheet.
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| CN109837061A (en) * | 2017-11-24 | 2019-06-04 | 洛阳尖端技术研究院 | Modified metal powder wave absorbing agent and preparation method thereof |
| CN111112601B (en) * | 2018-11-01 | 2021-10-01 | 哈尔滨工业大学 | High-temperature-resistant ferromagnetic wave absorbing agent, preparation method thereof and application of high-temperature-resistant ferromagnetic wave absorbing agent in preparation of high-temperature-resistant ferromagnetic wave absorbing material |
| CN113024237B (en) * | 2021-03-11 | 2022-06-03 | 深圳信义磁性材料有限公司 | Preparation method of magnetic nano composite material |
| CN114956828B (en) * | 2022-05-17 | 2023-08-15 | 合肥商德应用材料有限公司 | Silicon carbide ceramic and preparation method and application thereof |
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| CN101256863A (en) * | 2008-01-07 | 2008-09-03 | 北京化工大学 | Magnetic carrier of surface modification and preparing method thereof |
| KR20080088154A (en) * | 2007-03-29 | 2008-10-02 | 엘지마이크론 주식회사 | Magnetism nano particle coated silica and method for manufacturing thereof |
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| CN101388267B (en) * | 2008-07-09 | 2011-04-13 | 长春市博坤生物科技有限公司 | Silicon dioxide magnetic composite particle and preparation |
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| KR20080088154A (en) * | 2007-03-29 | 2008-10-02 | 엘지마이크론 주식회사 | Magnetism nano particle coated silica and method for manufacturing thereof |
| CN101256863A (en) * | 2008-01-07 | 2008-09-03 | 北京化工大学 | Magnetic carrier of surface modification and preparing method thereof |
| CN101613694A (en) * | 2009-05-31 | 2009-12-30 | 华东理工大学 | A kind of magnetic/functionalized SiO 2 composite microsphere immobilized enzyme and preparation method thereof |
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