CN109970457B - Low-temperature co-fired soft magnetic ferrite powder for laminated chip power inductor and preparation method thereof - Google Patents
Low-temperature co-fired soft magnetic ferrite powder for laminated chip power inductor and preparation method thereof Download PDFInfo
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Abstract
The formula of the low-temperature co-fired soft magnetic ferrite powder for the laminated chip power inductor comprises a base material and an additive, wherein the base material comprises Fe according to the mass ratio2O350.0-70.0% of NiO, 5.0-15.0% of NiO, 15-30.0% of ZnO and 3.84-9.40% of CuO3; additive, based on the total mass of the base material, Bi2O31.0-6.0% of clinker powder and 0.5-6.0% of clinker powder; wherein, the formula of the clinker comprises, by mass, 9-12% of alumina, 62-65% of silicon dioxide, 5-8% of calcium oxide, 0.5-1.0% of magnesium oxide, 2.0-4.0% of potassium oxide, 1.0-2.0% of sodium oxide and 8.0-10.0% of boron oxide. The base material is added with deionized water, stirred, mixed, dried and pre-sintered, and then the additive is added, mixed, dried and crushed. The powder material has reduced magnetic conductivity with the addition of additive and good DC bias resistance.
Description
Technical Field
The invention relates to ferrite powder, in particular to low-temperature co-fired soft magnetic ferrite powder for a laminated chip power inductor and a preparation method thereof.
Background
The laminated ferrite inductor has the excellent characteristics of small volume, low cost, excellent shielding performance, high reliability, easy surface mounting and the like, and is widely applied to the fields of mobile communication, computers, automotive electronics, televisions, broadcasting satellites and the like. In recent years, with the improvement of the transmission and processing speed of large data volume of electronic products, the power demand of chip inductor devices is increasing, so that higher technical requirements are put forward on the current resistance of the devices to meet the requirements of small size and high power. Especially in modern circuit systems, more and more electronic devices such as inductors, converters, beads, transformers, etc. are operated under low voltage and large current conditions, and the dc bias superposition characteristics of these devices have a great influence on the efficiency of the circuit system. Meanwhile, in some special practical circuit applications, the direct current superposition characteristics can have a great negative effect on the electromagnetic performance of the device, so that the research on the direct current bias characteristics of the laminated inductor is very important.
The rated current of the common laminated chip inductor is relatively small, only about 5-20 milliamperes, which can not meet the existing requirements, and the inductor needs to be designed to have the following characteristics: patch type, miniaturization and high rated current; comparing technical parameters with 2012-4.7 microhenry inductance, wherein the rated current of a common type is 10mA, the rated current of a heavy current type is 100mA, and the rated current of an ultra-large current type is 250 mA;
low-temperature co-firing characteristics: the inner coil of the laminated chip inductor adopts silver as an electrode, the sintering temperature of the material must be lower than 930 ℃, and the contraction and expansion curve of the silver needs to be matched, so that the ferrite material and the silver can be well combined, and the manufactured inductor can meet the requirements. Although the wire-wound chip inductor has a high current endurance value, the size is large, the production efficiency is low, and the cost is high.
The rated current of the laminated chip inductor is mainly determined by the thickness of a silver coil in the inductor, namely the larger the silver consumption is, the smaller the direct current resistance RDC of the coil is, and the higher the rated current of the inductor is; however, increasing the silver content brings the problem of co-firing and matching of the silver layer and the ferrite: gaps are formed between the magnets and the silver layer, and the magnets are cracked; therefore, there is an urgent need to develop a low-temperature co-fired soft magnetic ferrite with high current and high current-resistant characteristics, which relies on the high current-resistant characteristics of the material to increase the rated current of the device, reduce the amount of silver, and ensure the matching co-firing of silver and the magnet. At present, ferrite materials applied to laminated inductor devices are basically NiCuZn ferrite materials sintered at low temperature, so how to improve the magnetoelectric property and the direct current bias resistance of the NiCuZn ferrite materials sintered at low temperature by optimizing the formula of the materials, selecting proper dopants and selecting proper process conditions and methods is a problem to be solved urgently.
Disclosure of Invention
The invention aims to provide low-temperature co-fired soft magnetic ferrite powder for a laminated chip power inductor and a preparation method thereof.
In order to achieve the purpose, the technical scheme provided by the invention is that the low-temperature co-fired soft magnetic ferrite powder for the laminated chip power inductor comprises a base material and an additive according to the formula, wherein the base material comprises Fe according to the mass ratio2O350.0-70.0% of NiO, 5.0-15.0% of NiO, 15-30.0% of ZnO and 3.84-9.40% of CuO; additive, based on the total mass of the base material, Bi2O31.0-6.0% of fusion cake0.5-6.0% of powder; wherein, the formula of the clinker comprises, by mass, 9-12% of alumina, 62-65% of silicon dioxide, 5-8% of calcium oxide, 0.5-1.0% of magnesium oxide, 2.0-4.0% of potassium oxide, 1.0-2.0% of sodium oxide and 8.0-10.0% of boron oxide.
The invention also provides a preparation method of the low-temperature co-fired soft magnetic ferrite powder for the laminated chip power inductor, which comprises the following steps: 1) accurately weighing the components according to the proportion of the base material; 2) adding deionized water according to the weight ratio of the base material dry powder to the deionized water of 1:1.3, stirring and mixing to form base material slurry, wherein the granularity requirement D50 is 0.5-1.0 micron, and D90 is less than 2.0 micron; 3) drying the prepared base material slurry, wherein the water content is less than or equal to 0.6 percent after drying; 4) pre-burning the base material, namely pre-burning the dried base material at the temperature of 800-900 ℃, and preserving heat for 2-5 hours; 5) weighing the components of the additive according to the mass ratio of the additive based on the mass of the base material; 6) mixing the pre-sintered base material with an additive, adding deionized water according to the weight ratio of the mixed dry powder to the deionized water of 1:1.3, stirring and mixing, wherein the particle size requires that D50 is 0.5-1.0 micron, and D90 is less than 2.0 microns; 7) drying, wherein the water content after drying is less than or equal to 0.6 percent; 8) pulverizing and sieving to obtain the final product.
The drying temperature of the step 3) and the step 7) is 200-250 ℃.
Step 2) and step 6), mixing and ball-milling, and feeding: ball: the proportion of water is 3:1:1.3, the ball milling speed is 250 r/min, the ball milling mode is positively rotated for 30 min, and then is reversely rotated for 30 min.
And step 8), crushing and sieving by a 40-80 mesh sieve.
According to the invention, through optimization of the powder main body formula and adjustment of the component proportion of the additive, the flow resistance of the material is obviously improved, the influence on the magnetic conductivity of the material is small, the situation that the magnetic conductivity of the material is greatly reduced is avoided, and the performance of the powder is improved. The laminated inductor prepared from the nickel-copper-zinc ferrite powder introduces various elements into the powder through frit addition, so that the electromagnetic property of the powder is improved: permeability μ' 30-100(5MHz, 500 mV); quality factor: q is above 30 (5MHz, 500 mV); sintering temperature: less than 930 degrees; current impact: after the current impact of 5A, the change rate of the magnetic conductivity is less than 15 percent; d, direct current bias: and when the magnetic permeability is tested under the current of 3A, the change rate of the magnetic permeability is less than 35 percent.
Drawings
FIG. 1, permeability/quality factor vs. frequency curve for SL1/SL2/SL 3.
FIG. 2, SL1/SL2/SL3 impedance Z-frequency curve.
FIG. 3, permeability/quality factor vs. frequency curve for SL4/SL5/SL 6.
FIG. 4, SL4/SL5/SL6 impedance Z-frequency curve.
FIG. 5, permeability/quality factor vs. frequency curves for SL7/SL8
FIG. 6, SL7/SL8 impedance Z-frequency curve.
FIG. 7 shows the permeability-current impact curves for SL1/SL2/SL3/SL4/SL5/SL6/SL7/SL 8.
FIG. 8 shows the change curves of permeability-branch bias of SL1/SL2/SL3/SL4/SL5/SL6/SL7/SL8
Fig. 9, an electron micrograph of SL 1.
Fig. 10, an electron micrograph of SL 2.
Fig. 11, SL3 electron micrograph.
Fig. 12, an electron micrograph of SL 4.
Fig. 13, an electron micrograph of SL 5.
Fig. 14, an electron micrograph of SL 6.
Fig. 15, SL7 electron micrograph.
Fig. 16, SL8 electron micrograph.
Detailed Description
The purity requirements of the chemical reagents involved in the invention are as follows: iron (III) oxide Fe2O3More than or equal to 99.5 percent, nickel protoxide NiO more than or equal to 75 percent, copper oxide CuO more than or equal to 70 percent, zinc oxide ZnO more than or equal to 97 percent, bismuth trioxide Bi2O3≥99％。
The formula of the low-temperature co-fired soft magnetic ferrite powder comprises a base material and an additive: base material, by mass ratio, Fe2O350.0-70.0% of NiO, 5.0-15.0% of NiO, 15-30.0% of ZnO and 3.84-9.40% of CuO; additive, based on the total mass of the base material, Bi2O31.0-6.0% and 0.5-6.0% of clinker powder.
The frit formula of the frit powder comprises, by mass, 9-12% of alumina, 62-65% of silicon dioxide, 5-8% of calcium oxide, 0.5-1.0% of magnesium oxide, 2.0-4.0% of potassium oxide, 1.0-2.0% of sodium oxide and 8.0-10.0% of boron oxide.
The preparation method of the low-temperature co-fired soft magnetic ferrite powder comprises the following steps: 1) accurately weighing the components of the base material according to the proportion of the components of the base material; 2) adding deionized water according to the weight ratio of the base material dry powder to the deionized water of 1:1.3, stirring and mixing to form base material slurry, wherein the granularity requirement D50 is 0.5-1.0 micron, and D90 is less than 2.0 micron; 3) drying the prepared base material slurry, wherein the water content is less than or equal to 0.6 percent after drying; 4) pre-burning the base material, performing solid phase reaction on the dried base material to form a ferrite phase with uniform phase components, wherein the pre-burning temperature is 800-900 ℃, and the heat preservation is performed for 2-5 hours; 5) weighing a certain amount of the base stock after pre-sintering, and weighing the components of the additive according to the mass ratio of the components of the additive; 6) mixing the base material after pre-burning with the additive components, adding deionized water according to the weight ratio of the mixed dry powder to the deionized water of 1:1.3, stirring and mixing, wherein the granularity requires that D50 is 0.5-1.0 micron, and D90 is less than 2.0 micron; 7) drying the finished product, wherein the water content after drying is less than or equal to 0.6%; 8) pulverizing and sieving to obtain the final product. The drying temperature of the step 3) and the step 7) is 200 ℃ and 250 ℃.
The technical solution of the present invention will be described in detail below with reference to specific examples.
Table one: component ratios of examples 1 to 8
Table I shows the specific formulations of the base components and the additive components of examples 1 to 8, and the magnetic permeability of the inductor made of the powder prepared according to the formulations of examples 1 to 8 is in the range of 30 to 100. In actual production, the ferrite powder required by customers can be prepared by selecting a corresponding formula according to the magnetic conductivity required by the customers. Since the preparation processes of examples 1 to 8 are the same, the ingredients of the examples are weighed according to the ratio of table one, and then the preparation is performed by the same process steps.
The preparation method comprises the following steps:
1) weighing the base material according to the formula of each component of the base material in each example of the table I, and weighing an electronic scale with the precision of +/-1 g; the total weight of the ingredients is 200 g;
2) grinding the base material: putting the ingredients into a planetary milling jar for ball milling for 4 hours, and mixing: ball: the proportion of water is 3:1:1.3, the granularity D50 after ball milling is 0.5-1.0 micron, and D90 is less than 2.0 microns; the ball milling speed is 250 r/min, the ball milling mode positively rotates for 30 min, and then reversely rotates for 30 min;
3) drying the base material: drying the base material slurry subjected to ball milling in an electrothermal blowing drying oven at the drying temperature of 200 ℃ and 250 ℃ for 5 hours, wherein the water content after drying is less than or equal to 0.6 percent;
4) crushing and sieving the base material: after drying, crushing the base material by an electric crusher and sieving the base material by a 40-mesh sieve, and the aim is to improve the production efficiency;
5) pre-burning and crushing base materials: putting the ground base material powder into a corundum-mullite sagger for presintering; presintering by using a Nabo hot box type furnace, preserving heat for 5 hours at 900 ℃ for solid phase synthesis, and crushing by using an electric crusher after synthesis and sieving by using a 40-mesh sieve;
6) and (3) finished product batching: weighing 100 g of base material after presintering, crushing and sieving, weighing and adding according to the additive components and the proportion corresponding to each embodiment, and performing electronic scale precision: 0.01 g;
7) grinding the finished slurry: putting the base material and the additive into a planetary ball milling tank, adding deionized water to form finished slurry, carrying out wet ball milling for 6 hours at the rotating speed of 250 revolutions per minute, rotating forwards for 30 minutes, and then rotating backwards for 30 minutes; material preparation: ball: water ratio 3:1:1.3, D50 0.5-1.0 micron;
8) drying the finished slurry: drying the ball-milled finished slurry in an electrothermal blowing drying oven at the temperature of 200-250 ℃ for 5 hours until the water content is less than or equal to 0.6%;
9) crushing: and crushing the dried finished lump material by using an electric crusher and sieving the crushed lump material by using a 40-mesh sieve to obtain finished powder. In order to avoid the difference of performance among batches, the finished powder of multiple batches is uniformly packed and sold after being mixed in multiple batches of processing.
In the step 5), the pre-sintering temperature is 800-.
And step 5) pre-burning and crushing the base material and step 9), sieving the crushed base material, and generally controlling the number of the sieved meshes to be 40 meshes.
The formula of the frit in table one (in mass ratio) is as follows: 9-12% of aluminum oxide, 62-65% of silicon dioxide, 5-8% of calcium oxide, 0.5-1.0% of magnesium oxide, 2.0-4.0% of potassium oxide, 1.0-2.0% of sodium oxide and 8.0-10.0% of boron oxide. Before the base material is prepared, a frit is prepared. According to this formulation, for example: respectively weighing 11% of alumina, 65% of silicon dioxide, 7% of calcium oxide, 1% of magnesium oxide, 4% of potassium oxide, 2% of sodium oxide and 10% of boron oxide by mass ratio in a total amount of 500g, then uniformly stirring and mixing, putting into a smelting furnace for smelting at a smelting temperature of 950 ℃, naturally cooling to form a fusion cake after smelting, and then crushing the fusion cake to obtain the required fusion cake powder, wherein the particle size D50 of the fusion cake powder is less than or equal to 1.5 microns. Through the preparation of the frit, trace components which can be directly added into the base material originally, such as magnesium oxide, sodium oxide and potassium oxide, are added into the frit in a large amount, so that the weighing error is reduced, and the addition amount is more accurate. In addition, the frit is prepared in advance, so that the complexity of batching in the preparation of ferrite powder is saved, and the sintering temperature of the powder is reduced. As the frit contains a plurality of elements, the flow resistance and the direct current bias resistance of the ferrite powder can be effectively improved by increasing the addition amount of the frit.
In each embodiment, bismuth trioxide is added as a sintering aid to promote the growth of ferrite grains and improve the density of the magnet; when the ferrite powder manufactured by the invention is used for sintering the laminated chip inductor, the sintering temperature of the finished product is 900 ℃, and the low-temperature co-firing is realized.
The ferrite powder prepared in the above examples was subjected to a performance test experiment.
Firstly, manufacturing a testing magnetic ring: taking 10g of dry powder, adding a PVA adhesive with solid content of 3% for granulation, and enabling the specification of a die to be phi 20mm multiplied by phi 10 mm; forming size: outer diameter x inner diameter x thickness phi 20mm x phi 10mm is multiplied by 3 mm; green body density: 4.0 mm. + -. 0.1g/cm3(ii) a Forming by an automatic tabletting and forming machine, wherein the forming pressure is 10 MPa; inspecting the sintering temperature of the magnetic ring: and keeping the temperature at 900 +/-10 ℃ for 5 hours, and detecting by an imported ETH temperature measuring ring.
Table two, test methods and test items.
And performing performance test on the manufactured detection magnetic ring according to the test method and the test items in the table II. Test data are as shown in table three.
Third, test magnetic ring test data
According to the data, the electromagnetic performance parameters meet the target electromagnetic performance requirements. As can be seen from the data in the table, the magnetic permeability is gradually reduced along with the increase of the addition amount of the clinker powder, the current impact change is not large, but the direct current bias is obviously improved, the density of the magnet is slightly reduced, and the requirement of dense sintering can still be met.
As can be seen from the analysis data and the graphs, the quality factor is not obviously changed along with the increase of the clinker powder, the self-resonant frequency is improved, the direct current bias performance is greatly improved, and meanwhile, the magnetic permeability can be kept to 100. The common ferrite powder has the magnetic conductivity of 100, the bias characteristic under the condition of 3A is as high as 65%, and the bias characteristic of the powder material of the invention is less than 35%, thus the ferrite powder material of the invention has excellent direct current bias resistance.
Claims (6)
1. The formula of the low-temperature co-fired soft magnetic ferrite powder for the laminated chip power inductor comprises a base material and an additive, wherein the base material comprises Fe according to the mass ratio2O350.0-70.0% of NiO, 5.0-15.0% of NiO, 15-30.0% of ZnO and 3.84-9.40% of CuO3; additive, based on the total mass of the base material, Bi2O31.0-6.0% of clinker powder and 0.5-6.0% of clinker powder; wherein the frit isThe formula comprises, by mass, 9-12% of alumina, 62-65% of silicon dioxide, 5-8% of calcium oxide, 0.5-1.0% of magnesium oxide, 2.0-4.0% of potassium oxide, 1.0-2.0% of sodium oxide and 8.0-10.0% of boron oxide, wherein the sum of the components of the clinker is 100%.
2. The method for preparing the low-temperature co-fired soft magnetic ferrite powder for the laminated chip power inductor according to claim 1, comprising the steps of: 1) accurately weighing the components according to the proportion of the base material; 2) adding deionized water into the weighed and mixed base material dry powder, stirring and mixing to form base material slurry, wherein the granularity requirement D50=0.5-1.0 micron, and D90 is less than 2.0 microns; 3) drying the prepared base material slurry, wherein the water content is less than or equal to 0.6 percent after drying; 4) pre-burning the base material, namely pre-burning the dried base material at the temperature of 800-900 ℃, and preserving heat for 2-5 hours; 5) weighing the components of the additive according to the mass ratio of the additive based on the mass of the base material; 6) mixing the pre-sintered base material with the additive, adding deionized water, stirring and mixing, wherein the particle size is required to be D50=0.5-1.0 micron, and D90 is less than 2.0 microns; 7) drying the finished product, wherein the water content after drying is less than or equal to 0.6%; 8) pulverizing and sieving to obtain the final product.
3. The method for preparing the low-temperature co-fired soft magnetic ferrite powder for the laminated chip power inductor as claimed in claim 2, wherein the drying temperature in the steps 3) and 7) is 200-250 ℃.
4. The method for preparing the low-temperature co-fired soft magnetic ferrite powder for the laminated chip power inductor according to claim 2, wherein the steps 2) and 6) are respectively ball-milled and mixed, and the materials are as follows: ball: the water ratio =3:1:1.3, the ball milling speed is 250 r/min, the ball milling mode is rotated forwards for 30 min, and then is rotated backwards for 30 min.
5. The method for preparing low-temperature co-fired soft magnetic ferrite powder for the laminated chip power inductor according to claim 2, wherein the step 8) is carried out by pulverizing and sieving with 40-80 meshes.
6. The method for preparing low-temperature co-fired soft magnetic ferrite powder for the laminated chip power inductor according to claim 2, wherein the preparation method of the frit powder comprises the steps of weighing each component of the frit according to a formula based on the total mass of prepared frit ingredients, uniformly mixing, melting, cooling, and crushing to prepare the frit powder for later use.
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