CN109970457A - Lamination sheet type power inductor low temperature co-fired soft ferromagnetic powder and preparation method thereof - Google Patents

Lamination sheet type power inductor low temperature co-fired soft ferromagnetic powder and preparation method thereof Download PDF

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CN109970457A
CN109970457A CN201910307835.4A CN201910307835A CN109970457A CN 109970457 A CN109970457 A CN 109970457A CN 201910307835 A CN201910307835 A CN 201910307835A CN 109970457 A CN109970457 A CN 109970457A
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base
powder
additive
frit
low temperature
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CN109970457B (en
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邹文轩
邹家昊
邹家轩
刘润生
曹淑松
曹卜文
程倩雯
赵远东
左冬阳
杜亚男
杜欣洁
邹金彪
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Linyi Chenghe Information Technology Co Ltd
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Abstract

Lamination sheet type power inductor low temperature co-fired soft ferromagnetic powder and preparation method thereof, formula include base-material and additive, wherein base-material, in mass ratio, Fe2O350.0~70.0%, NiO 5.0~15.0%, ZnO15~30.0%, CuO3.84~9.40%;Additive, in terms of base-material gross mass, Bi2O31.0~6.0%, frit powder 0.5~6.0%;Wherein, the formula of frit is aluminium oxide 9-12%, silica 62-65%, calcium oxide 5-8%, magnesia 0.5-1.0%, potassium oxide 2.0-4.0%, sodium oxide molybdena 1.0-2.0%, boron oxide 8.0-10.0% by quality ratio.It is stirred pre-burning after drying by base-material plus deionized water, then adds additive and deionized water mixing dries pulverizing is added.The powder is reduced as magnetic conductivity is added in additive, and anti-direct current biasing performance is good.

Description

Lamination sheet type power inductor low temperature co-fired soft ferromagnetic powder and its preparation Method
Technical field
The present invention relates to ferrite powders, refer in particular to lamination sheet type power inductor with low temperature co-fired soft magnetic ferrite powder Material and preparation method thereof.
Background technique
Lamination sheet type ferrite inductance device is small in size, at low cost by its, shielding properties is excellent, high reliablity, is easy to It realizes the excellent characteristics such as Surface Mount dress, obtains in fields such as mobile communication, computer, automotive electronics, TV, broadcasting satellites and answer extensively With.In recent years, with the transmission of electronic product big data quantity and the raising of processing speed, to the power demand of chip inductor device Also increasing, therefore higher technical requirements are proposed to the withstanding current capability of the device, it is powerful to meet small size It is required that.Especially in modern circuitry, the works such as more and more electronic equipments such as inductor, converter, magnetic bead, transformer Make under the conditions of low-voltage, high-current, the direct current biasing superimposed characteristics of these devices have very big shadow to the efficiency of circuit system It rings.Simultaneously in some special actual circuit applications, DC superposition characteristic can generate very big bear to the electromagnetic performance of device Face is rung, therefore is also particularly important to the research of the direct current biasing characteristic of laminated inductive.
The rated current of normal stack chip inductor is smaller, only 5-20 milliamperes or so, is not able to satisfy existing requirement, Patch type, miniaturization, high rated current should be had the following characteristics that by needing to design a inductor;With 2012-4.7 microhenry electricity Feel correlation technique parameter, medium-sized rated current is 10mA, the rated current 100mA of high current type, the volume of super-large current type Constant current 250mA;
Low temperature co-fired characteristic: laminated chip inductor Inside coil is used as electrode using silver, and material sintering temperature must be low It in 930 degree, and needs to match the convergent-divergent curve of silver, can be only achieved the good combination of Ferrite Material and silver, production Inductor can just be met the requirements.Although coiling SMT Inductor has high resistance to flow valuve, its size is big, and production efficiency is low, at This height.
What the rated current of laminated chip inductor was mainly determined by the thickness of silver wire circle inside inductor, that is, silver Dosage is bigger, and the D.C. resistance RDC of coil is smaller, and the rated current of inductor is also higher;But increase the content of silver simply The problem of bringing silver layer and ferrite co-fire match again: magnet and silver layer have the gap, magnet cracking;So being badly in need of developing one kind The low temperature co-fired soft magnetic ferrite of the high resistance to properties of flow of high current, the specified electricity of device is promoted by the resistance to properties of flow of height of material Stream reduces the dosage of silver, it is ensured that the matching co-firing of silver and magnet.Currently, the ferrite material applied in lamination type electric inductor component Material is substantially using low sintering NiCuZn Ferrite Material, therefore, how suitable by the formula of optimization material, selection Dopant, the suitable process conditions of selection and method improve the magnetic electricity performance of low-temperature sintering NiCuZn Ferrite Material and anti- Direct current biasing characteristic becomes problem in the urgent need to address.
Summary of the invention
The object of the present invention is to provide a kind of low temperature co-fired soft ferromagnetic powder of lamination sheet type power inductor and its Preparation method, ferrite powder preparation laminated chip inductor may be implemented patch type, miniaturization, high rated current, And the superior electricals performance such as better anti-direct current biasing characteristic.
To achieve the above object, technical solution provided by the invention is the low temperature co-fired soft magnetism of lamination sheet type power inductor Ferrite powder, formula include base-material and additive, wherein base-material, in mass ratio, Fe2O350.0~70.0%, NiO 5.0~15.0%, ZnO 15~30.0%, CuO 3.84~9.40%;Additive, in terms of base-material gross mass, Bi2O31.0~ 6.0%, frit powder 0.5~6.0%;Wherein, the formula of frit is aluminium oxide 9-12%, silica 62- by quality ratio 65%, calcium oxide 5-8%, magnesia 0.5-1.0%, potassium oxide 2.0-4.0%, sodium oxide molybdena 1.0-2.0%, boron oxide 8.0- 10.0%.
The present invention also provides the lamination sheet type power inductor preparation method of low temperature co-fired soft ferromagnetic powder, Step includes: 1) accurately to weigh according to the proportion of base-material each component;2) according to the weight ratio 1:1.3 of base-material dry powder and deionized water Deionized water is added, is stirred to form base-material slurry, D50=0.5-1.0 microns of granularity requirements, D90 is less than 2.0 microns;3) The base-material slurry of preparation is dried, water content≤0.6% after drying;4) base-material pre-burning, by the base-material pre-burning after drying, 800-900 DEG C of calcined temperature, keep the temperature 2-5 hours;5) in terms of base-material quality, according to additive mass ratio, additive each group is weighed Part;6) base-material after pre-burning is mixed with additive, according to the weight ratio addition of dry powder after mixing and deionized water 1:1.3 go from Sub- water is stirred, and D50=0.5-1.0 microns of granularity requirements, D90 is less than 2.0 microns;7) it dries, water content after drying≤ 0.6%;8) it pulverizes and sieves to obtain finished product.
The drying temperature 200-250 degree of the step 3) and step 7).
Step 2) and step 6) mixing and ball milling, material: ball: water ratio=3:1:1.3,250 revs/min of rotational speed of ball-mill, ball milling Mode rotates forward 30 minutes, then inverts 30 minutes.
Step 8) pulverizes and sieves mesh number as 40-80 mesh.
The present invention makes the resistant to flow spy of material by the adjustment of the proportioning components of optimization and additive to powder main body formula Property be improved significantly, while on the magnetic conductivity of material itself influence it is smaller, permeability sharp fall will not be generated Situation improves the performance of powder.The inductor of the lamination sheet type of nickel copper zinc ferrite powder preparation of the invention, passes through frit Addition, multiple element is introduced in powder, improves the electromagnetic performance of powder: magnetic permeability μ '=30-100 (5MHz, 500mV);Product Prime factor: Q is in 30 or more (5MHz, 500mV);Sintering temperature: it is lower than 930 degree;Rush of current: after 5A rush of current, magnetic conductivity Change rate is less than 15%;Direct current biasing: testing under 3A electric current, and magnetic conductivity change rate is less than 35%.
Detailed description of the invention
Fig. 1, SL1/SL2/SL3 magnetic conductivity/quality factor -- frequency curve.
Fig. 2, SL1/SL2/SL3 impedance Z -- frequency curve.
Fig. 3, SL4/SL5/SL6 magnetic conductivity/quality factor -- frequency curve.
Fig. 4, SL4/SL5/SL6 impedance Z -- frequency curve.
Fig. 5, SL7/SL8 magnetic conductivity/quality factor -- frequency curve
Fig. 6, SL7/SL8 impedance Z -- frequency curve.
Fig. 7, SL1/SL2/SL3/SL4/SL5/SL6/SL7/SL8 magnetic conductivity-rush of current curve.
Fig. 8, SL1/SL2/SL3/SL4/SL5/SL6/SL7/SL8 magnetic conductivity-tributary offset change curve
Fig. 9, SL1 electromicroscopic photograph.
Figure 10, SL2 electromicroscopic photograph.
Figure 11, SL3 electromicroscopic photograph.
Figure 12, SL4 electromicroscopic photograph.
Figure 13, SL5 electromicroscopic photograph.
Figure 14, SL6 electromicroscopic photograph.
Figure 15, SL7 electromicroscopic photograph.
Figure 16, SL8 electromicroscopic photograph.
Specific embodiment
The present invention relates to chemical reagent purity requirement: di-iron trioxide Fe2O3>=99.5%, nickel protoxide NiO >= 75%, copper oxide CuO >=70%, zinc oxide ZnO >=97%, bismuth oxide Bi2O3>=99%.
The formula of low temperature co-fired soft magnetic ferrite powder of the invention includes base-material and additive: base-material, in mass ratio, Fe2O350.0~70.0%, NiO 5.0~15.0%, ZnO 15~30.0%, CuO 3.84~9.40%;Additive, with base Expect gross mass meter, Bi2O31.0~6.0%, frit powder 0.5~6.0%.
The frit formula of frit powder, each component is according to mass ratio, aluminium oxide 9-12%, silica 62-65%, calcium oxide 5-8%, magnesia 0.5-1.0%, potassium oxide 2.0-4.0%, sodium oxide molybdena 1.0-2.0%, boron oxide 8.0-10.0%.
1) preparation method of low temperature co-fired soft magnetic ferrite powder of the invention includes the following steps: according to base-material each component Proportion accurately weigh base-material each component;2) deionized water is added according to base-material dry powder and the weight ratio 1:1.3 of deionized water, into Row is stirred to form base-material slurry, and D50=0.5-1.0 microns of granularity requirements, D90 is less than 2.0 microns;3) by the base-material of preparation Slurry drying, water content≤0.6% after drying;4) the base-material pre-burning after drying is carried out solid phase reaction, is formed by base-material pre-burning Object phase composition uniform ferrite phase, keeps the temperature 2-5 hours by 800-900 DEG C of calcined temperature;5) base after a certain amount of pre-burning is weighed Material, weighs additive each component according to the mass ratio of additive each component;6) base-material after pre-burning is mixed with additive each component, Deionized water is added according to the weight ratio of dry powder after mixing and deionized water 1:1.3 to be stirred, granularity requirements D50=0.5- 1.0 microns, D90 is less than 2.0 microns;7) finished product drying, moisture content≤0.6% after drying;8) it pulverizes and sieves to obtain finished product.Step It is rapid 3) and the drying temperature 200-250 degree of step 7).
Carry out the technical solution that the present invention will be described in detail below by way of specific embodiment.
Table one: each group distribution ratio of embodiment 1 to embodiment 8
Table one is embodiment 1 to the base-material each component of embodiment 8 and the specific formula of additive each component, according to embodiment The permeability range of inductor made of 1 powder prepared to the formula of embodiment 8 is 30 to 100.In actual production, may be used The magnetic conductivity according to needed for client, ferrite powder needed for selecting corresponding formula preparation client.Due to embodiment 1 to implementation The process of preparing of example 8 is identical, thus, it is only required to the ingredient of each embodiment be weighed according to the proportion of table one, then by identical Processing step preparation.
It is specific the preparation method is as follows:
1) according to the base-material each component formula of each embodiment of table one, base-material is weighed, weighs electronic scale precision ± 1 gram;Match Material total weight is 200g;
2) base-material is ground: ingredient being put into ball milling 4 hours in planetary mills ball grinder, is expected: ball: water ratio=3:1:1.3, ball Granularity D50=0.5-1.0 microns after mill, D90 is less than 2.0 microns;250 revs/min of rotational speed of ball-mill, ball milling method rotates forward 30 points Then clock inverts 30 minutes;
3) base-material is dried: base-material slurry is dried by electric drying oven with forced convection after ball milling, and drying temperature selects 200-250 DEG C, the time 5 hours, moisture content≤0.6% after drying;
4) base-material pulverizes and sieves: base-material crosses 40 meshes using electronic broken crusher machine after drying, and the purpose is to improve production Efficiency;
5) base-material pre-burning crushes: smashed base-material powder being put into corundum-mullite sagger and carries out pre-burning;Pre-burning is selected Na Bore batch-type furnace, 900 degree of temperature heat preservations, 5 hours progress synthesis in solid state cross 40 meshes using electronic broken crusher machine after synthesis;
6) finished product ingredient: weighing 100 grams of the base-material after pre-burning pulverizes and sieves, according to the corresponding additive group of each embodiment Part and ratio carry out weighing addition, electronic scale precision: ± 0.01 gram;
7) finished pulp abrasive lapping: being put into planetary ball mill tank for base-material and additive, and deionized water is added and forms finished product slurry, It carries out wet ball-milling 6 hours, 250 revs/min of revolving speed, rotates forward 30 minutes, then invert 30 minutes;Material: ball: water ratio=3:1: 1.3, D50=0.5-1.0 microns;
8) finished product slurry is dried: the finished product slurry after ball milling being dried by electric drying oven with forced convection, drying temperature selection 200 DEG C~250 DEG C, drying time 5 hours, moisture content≤0.6% after drying;
9) it crushes: the finished product block after drying being crossed into 40 meshes using electronic broken crusher machine, obtains finished product powder.In order to Performance difference is avoided between batch, in multiple batches of processing, uniform packing is sold again after multiple batches of finished product powder is mixed.
In above-mentioned steps 5) base-material pre-burning crush in, 800-900 DEG C of calcined temperature, soaking time control at 2-5 hours.
In step 5) base-material pre-burning crushing and step 9), grinding and sieving crosses grit number general control in 40 mesh.
The formula of frit in table one (with mass ratio) are as follows: aluminium oxide 9-12%, silica 62-65%, calcium oxide 5- 8%, magnesia 0.5-1.0%, potassium oxide 2.0-4.0%, sodium oxide molybdena 1.0-2.0%, boron oxide 8.0-10.0%.In base-material system Before standby, frit need to be first prepared.According to the formula, citing: in terms of total amount 500g, according to aluminium oxide 11%, silica 65%, Calcium oxide 7%, magnesia 1%, potassium oxide 4%, sodium oxide molybdena 2%, boron oxide 10% mass ratio weigh each component respectively, then It is uniformly mixed, is put into smelting furnace and melts, 950 DEG C of melting temperature, natural cooling is at frit again after melting, then by frit powder It is broken that required frit powder, frit Powder Particle Size D50≤1.5 micron are made.By the preparation of frit, script can be added directly into base Trace Components in material, such as magnesia, sodium oxide molybdena, potassium oxide are added in frit in the form of larger quantities, reduce weighing Error, keep additive amount more acurrate.In addition, preparing in advance by frit, saves the ingredient in ferrite powder preparation Sintering temperature that is cumbersome and reducing powder.Since frit contains multiple element, the increase of the additive amount of frit can be mentioned effectively The resistance to properties of flow of liter ferrite powder and anti-direct current biasing characteristic.
In the above embodiments, addition bismuth oxide promotes ferrite crystal grains growth, improves magnet as sintering aid Consistency;When being sintered laminated chip inductor using the ferrite powder that the present invention makes, finished product sintering temperature is 900 DEG C, It realizes low temperature co-fired.
Experiment is tested for the property to the ferrite powder that above-described embodiment is prepared.
Magnet ring is examined in production first: taking 10g dry powder, the adhesive that solid content 3%PVA is added is granulated, mould specification Φ 20mm×Φ10mm;Compact dimensions: outer diameter × internal diameter × thickness=Φ 20mm × Φ 10mm × 3mm;Blank density: 4.0mm ± 0.1g/cm3;Automatic tabletting forming machine molding, briquetting pressure 10MPa;Examine magnet ring sintering temperature: 900 ± 10 DEG C, heat preservation 5 is small When, the detection of import ETH firing ring.
Table two, test method and test item.
The detection magnet ring of production is tested for the property according to the test method of table two and test item.Test data such as table Three.
Table three examines magnet ring test data
From the above data, electromagnetic performance parameter is all satisfied purpose electromagnetic performance requirement.And from the data in the table, with The increase of such frit powder additive amount, magnetic conductivity gradually decrease, less, but direct current biasing obtains obviously for rush of current variation Improve, magnet density slightly reduces, but still can satisfy the requirement of dense sintering.
By analysis data and figure it is found that with frit powder increase, quality factor do not have significant change, self-resonant frequency It improves, while direct current biasing performance significantly improves, magnetic conductivity is able to maintain to 100.Ordinary ferrite powder, magnetic conductivity 100, Biasing characteristic under 3A is up to 65%, and the biasing characteristic of powder of the present invention illustrates ferrite powder of the invention less than 35% Anti- direct current biasing is had excellent performance.

Claims (6)

1. the low temperature co-fired soft ferromagnetic powder of lamination sheet type power inductor, formula includes base-material and additive, wherein Base-material, in mass ratio, Fe2O350.0~70.0%, NiO 5.0~15.0%, ZnO 15~30.0%, CuO 3.84~ 9.40%;Additive, in terms of base-material gross mass, Bi2O31.0~6.0%, frit powder 0.5~6.0%;Wherein, the formula of frit For by quality ratio, aluminium oxide 9-12%, silica 62-65%, calcium oxide 5-8%, magnesia 0.5-1.0%, potassium oxide 2.0-4.0%, sodium oxide molybdena 1.0-2.0%, boron oxide 8.0-10.0%.
2. the preparation side of the low temperature co-fired soft ferromagnetic powder of lamination sheet type power inductor according to claim 1 Method, step include: 1) accurately to weigh according to the proportion of base-material each component;2) in weighing mixed base-material dry powder addition go from Sub- water is stirred to form base-material slurry, and D50=0.5-1.0 microns of granularity requirements, D90 is less than 2.0 microns;3) by preparation The drying of base-material slurry, water content≤0.6% after drying;4) base-material pre-burning, by the base-material pre-burning after drying, calcined temperature 800- 900 DEG C, keep the temperature 2-5 hours;5) in terms of base-material quality, according to additive mass ratio, additive each component is weighed;It 6) will be after pre-burning Base-material is mixed with additive, and deionized water is added and is stirred, D50=0.5-1.0 microns of granularity requirements, D90 is micro- less than 2.0 Rice;7) finished product drying, water content≤0.6% after drying;8) it pulverizes and sieves to obtain finished product.
3. the preparation side of the low temperature co-fired soft ferromagnetic powder of lamination sheet type power inductor according to claim 2 Method, it is characterised in that the drying temperature 200-250 degree of the step 3) and step 7).
4. the preparation side of the low temperature co-fired soft ferromagnetic powder of lamination sheet type power inductor according to claim 2 Method, it is characterised in that step 2) and step 6) mixing and ball milling, material: ball: water ratio=3:1:1.3,250 revs/min of rotational speed of ball-mill, Ball milling method rotates forward 30 minutes, then inverts 30 minutes.
5. the preparation side of the low temperature co-fired soft ferromagnetic powder of lamination sheet type power inductor according to claim 2 Method, it is characterised in that step 8) pulverizes and sieves mesh number as 40-80 mesh.
6. the preparation side of the low temperature co-fired soft ferromagnetic powder of lamination sheet type power inductor according to claim 2 Method, it is characterised in that the preparation method of the frit powder is, to prepare in terms of frit ingredient gross mass, according to formula, to weigh respectively Frit each component, melts after mixing, then cools down, then crush that frit powder is made is spare.
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