CN104392820B - Composite soft magnetic material and preparation method thereof - Google Patents
Composite soft magnetic material and preparation method thereof Download PDFInfo
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- CN104392820B CN104392820B CN201410214841.2A CN201410214841A CN104392820B CN 104392820 B CN104392820 B CN 104392820B CN 201410214841 A CN201410214841 A CN 201410214841A CN 104392820 B CN104392820 B CN 104392820B
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Abstract
The invention discloses a composite soft magnetic material and a preparation method thereof. The composite soft magnetic material comprises the following components in percentage by weight: 75.13 to 86.12 percent of FeSiCr alloy powder, 9-14.5 percent of Fe2O3, 1.95-2.99 percent of NiO, 2.15-3.75 percent of ZnO, 0.55-1.43 percent of CuO, 0.03-0.85 percent of Bi2O3, 0.15-0.45 percent of V2O5 and 0.05-0.9 percent of SiO2. During preparation, the components are prepared, and the composite soft magnetic material is obtained by mixing, pre-burning, smashing, pressing and sintering. According to the composite soft magnetic material and the preparation method thereof disclosed by the invention, components of specific mixture ratio content are adopted, so that the composite soft magnetic material with high insulation, high pressure resistance and high Bs performance is prepared through the adjustment of the content of each material or adding of certain components in cooperation with a production process.
Description
【Technical field】
The present invention relates to soft magnetic materials, more particularly to a kind of compound soft magnetic material and preparation method thereof.
【Background technology】
Soft magnetic materials is usually used in the magneticss such as magnetic core of transformer, choking-winding or magnetic head.As device is to small-sized
Change and high current direction is developed, the performance of soft magnetic materials is put forward higher requirement.Existing soft magnetic materials is typically with ferrum
Oxysome is main component, including Fe2O3, NiO, ZnO, CuO and SiO2.The existing soft magnetic materials is being applied to some magnetic units
Some shortcomings are occurred in that during part.For example, when soft magnetic materials is applied in power inductor, power inductor is made in high frequency
With, especially in 100KHz and used above, one side magnetically soft alloy material often due to resistivity is relatively low, insulation and resistance to pressure
Can be relatively low, core heating is larger, causes the penalty of device.Another aspect soft magnetic ferrite is due to saturation flux density
(Bs) it is relatively low, cause the direct current biasing characteristic of power inductance device not enough.Therefore, it is the miniaturization and big electricity that adapt to device
The demand for development of fluidisation, exploitation are very necessary with the high Bs compound soft magnetic materials of high insulation high withstand voltage.
【The content of the invention】
The technical problem to be solved is：Above-mentioned the deficiencies in the prior art are made up, a kind of composite soft-magnetic material is proposed
Material and preparation method thereof, compound soft magnetic material have the performance of the high Bs of high insulation high withstand voltage.
The technical problem of the present invention is solved by following technical scheme：
A kind of compound soft magnetic material, material include the component of following percentage by weight：75.13～86.12wt%'s
The Fe of FeSiCr alloy powders, 9～14.5wt%2O3, the NiO of 1.95～2.99wt%, the ZnO of 2.15～3.75wt%, 0.55
The Bi of the CuO of～1.43wt%, 0.03～0.85wt%2O3, 0.15～0.45wt% V2O5, 0.05～0.9wt% SiO2。
A kind of manufacture method of compound soft magnetic material, according to the component proportion dispensing of following percentage by weight：75.13～
The FeSiCr alloy powders of 86.12wt%, the Fe of 9～14.5wt%2O3, 1.95～2.99wt% NiO, 2.15～
The ZnO of 3.75wt%, the CuO of 0.55～1.43wt%, the Bi of 0.03～0.85wt%2O3, 0.15～0.45wt% V2O5、
The SiO of 0.05～0.9wt%2；By the dispensing after mixing, pre-burning, crushing, pelletize, compacting and sintering, it is obtained described multiple
Close soft magnetic materials.
The beneficial effect that the present invention is compared with the prior art is：
It is in compound soft magnetic material of the present invention and preparation method thereof, using the component of specific proportioning content, each so as to pass through
The content adjustment of material or the addition of some components, cooperated technique for producing are obtained with the high Bs performances of high insulation high withstand voltage
Compound soft magnetic material.Experiments verify that, obtained in the present invention, the performance of compound soft magnetic material is：Initial permeability μ i is 50 (1
± 20%), and saturation induction density Bs >=900mT, insulation resistance >=100M Ω, pressure >=100V.It is of the invention obtained compound
The characteristics of soft magnetic materials has high insulation pressure and high Bs, the miniaturization of adaptation magnetic device and high current are to soft magnetic materials
Require.
【Description of the drawings】
Fig. 1 is the flow chart of the manufacture method of compound soft magnetic material in the specific embodiment of the invention；
Fig. 2 is the contrast curve that experimental example 1 in the specific embodiment of the invention and comparative example power up properties of flow.
【Specific embodiment】
With reference to specific embodiment and compare accompanying drawing the present invention is described in further details.
A kind of compound soft magnetic material, a kind of height of initial permeability for 50 (1 ± 20%) is proposed in this specific embodiment
The insulation high Bs compound soft magnetic materials of high withstand voltage, with it is high insulate pressure and high powered stream the characteristics of, adaptation power inductance it is little
The requirement of type and high current to soft magnetic materials.Compound soft magnetic material includes the component of following percentage by weight：75.13～
The FeSiCr alloy powders of 86.12wt%, the Fe of 9～14.5wt%2O3, 1.95～2.99wt% NiO, 2.15～
The ZnO of 3.75wt%, the CuO of 0.55～1.43wt%, the Bi of 0.03～0.85wt%2O3, 0.15～0.45wt% V2O5、
The SiO of 0.05～0.9wt%2。
In above-mentioned formula, saturation induction density Bs of material is adjusted by the content of adjustment FeSiCr powder.Pass through
Adjustment Fe2O3The content of NiO ZnO CuO come the ferritic contents of NiCuZn that adjust generation, so as to improve the pcrmeability of material
With the insulation and pressure performance for increasing material.By increasing SiO2Content be conducive to further improving the insulation of material and pressure
Performance.Add Bi2O3And V2O5Sintering temperature is reduced during manufacture process can be conducive to.Above-mentioned recipe ingredient, cooperated technique for producing can
Material crystalline distribution is adjusted further, so as to obtain the soft magnetic materials of preferably insulation and voltage endurance.
Preferably, the mean diameter of FeSiCr alloy powders is 3～30 μm, and remaining component is nano material, and particle diameter is
50～100nm.By the size controlling of each component in the scope, be conducive to the abundant reaction between various powders, can cause compound
Crystallization in soft magnetic materials is more uniform.
A kind of manufacture method of compound soft magnetic material is proposed in this specific embodiment, as shown in figure 1, for manufacture method
Flow chart, comprises the steps：Percentage by weight and component proportion dispensing as described above, by dispensing through mixing,
Pre-burning, crushing, pelletize, compacting and sintering, are obtained compound soft magnetic material.
Preferably, carry out according to following concrete steps：
1) when mixing, dry mixed is carried out, incorporation time is 60～90 minutes.
2) material for mixing under nitrogen protection atmosphere is carried out pre-burning and obtains Preburning material, calcined temperature control by pre-burning
At 700 ± 20 DEG C, burn-in time is 200～300 minutes, and during pre-burning, Control for Oxygen Content is below 1%.In the step, can push away
Pre-burning is carried out in plate kiln.
3) crush：By the step 2) Preburning material that obtains carries out waterproof pulverization, with dehydrated alcohol as solvent during crushing, powder
The broken time is 60～120 minutes, controls slip particle diameter at 3～30 μm after crushing.
4) pelletize：The tree for dissolving in dehydrated alcohol equivalent to the 3～4% of the slip weight is added in the slip
Fat binding agent, protects mist projection granulating using nitrogen, obtains particulate material.In the step, can select furfural resin as herein can
It is dissolved in the resinoid bond of dehydrated alcohol.
5) suppress：Obtain blank by the particulate material compressing, the pressed density control of the blank (5.55 ±
0.10)g/cm3.In the step, blank can be obtained by the particulate material compressing using powder former.
6) sinter：The blank is sintered under nitrogen protection atmosphere, for example, can be sintered in resistance furnace, burnt
Junction temperature is controlled at 750 DEG C～790 DEG C, and during sintering, Control for Oxygen Content is below 1%；200～300 minutes are incubated after sintering, with
After be cooled to room temperature, be obtained the compound soft magnetic material.
Compound soft magnetic material obtained in this concrete mode, initial permeability are 50 (1 ± 20%), high resistance to high insulation
The performance of high Bs is pressed, the requirement of the miniaturization and high current of magnetic device to soft magnetic materials is adapted to.This specific embodiment
Manufacture method, whole manufacturing processes are simple and easy to control, are conducive to industrialized production.
It is following by experimental example is set and comparative example verify the insulation of compound soft magnetic material obtained in manufacture method it is pressure with
And the performance such as magnetic induction.
Experimental example 1～5：According to the dispensing of each experimental example of recipe ingredient proportioning as shown in table 1, the good dispensing of proportioning is entered
Row dry mixed, incorporation time are 75 minutes.The material for mixing is carried out into pre-burning under nitrogen protection atmosphere and obtains Preburning material,
At 700 DEG C, burn-in time is 250 minutes for calcined temperature control, and during pre-burning, Control for Oxygen Content is 0.8%.By the Preburning material for obtaining
Waterproof pulverization is carried out, with dehydrated alcohol as solvent during crushing, grinding time is 90 minutes, and slip size controlling is in 16 μ after crushing
m.The furfural resin equivalent to the 3.5% of the slip weight is added in the slip, mist projection granulating is protected using nitrogen, is obtained
To particulate material.Blank is obtained by the particulate material compressing, the pressed density of the blank is controlled in 5.55g/cm3.By institute
State blank to be sintered under nitrogen protection atmosphere, sintering temperature is controlled at 770 DEG C, during sintering, Control for Oxygen Content is burnt 0.8%
250 minutes are incubated after knot, room temperature is then cooled to, the compound soft magnetic material is obtained.For ease of test, by compound soft magnetic material
Make composite magnet ring sample (T8 × 5 × 2).
Comparative example：According to the dispensing in recipe ingredient proportioning comparative example shown in table 1, composite soft-magnetic is obtained using traditional handicraft
Material.Equally, for ease of test, compound soft magnetic material is made into composite magnet ring sample (T8 × 5 × 2).
Reference example 1～4：For verifying recipe ingredient specificity in determination process in this specific embodiment, reference is set
Example, saves some components, and whether product obtained in checking still has the performance of the high Bs of high insulation high withstand voltage.According to 1 institute of table
Show the dispensing in recipe ingredient proportioning reference example 1～4, using and experimental example identical technique compound soft magnetic material is obtained.Equally,
For ease of test, compound soft magnetic material is made into composite magnet ring sample (T8 × 5 × 2).
Table 1
Obtained composite magnet ring is tested respectively and evaluated.Under the conditions of number of turn N=26Ts, using HP-
4284 type LCR testers test the initial permeability μ i of magnet ring sample；With the saturation of SY-8218 type B-H analyser test samples
Magnetic induction density B s；With insulation and the pressure performance of CH-333 types insulation Hi-pot Tester test sample.The result that test is obtained
As shown in table 2.
Table 2 (more than additional " * " of lower specification limit)
Knowable to the test data of table 2, the experimental example 1～5 of this specific embodiment compares with comparative example, and this is concrete real
Apply mode and there is preferably insulation and pressure performance, and corresponding initial permeability 50 (1 ± 20%), higher saturation can be kept
Magnetic induction.The compound soft magnetic material of this specific embodiment should be able to meet the miniaturization of power inductance and high current
Requirement to soft magnetic materials.And contrast experiment's example and reference example understand, after saving some components, product some or it is a few
Individual performance will be unable to meet, and will lack no relatedness between which performance with regard to saving which component, so determining this
The component and content of specific embodiment needs to do more work.
In addition, for the Bs of observation product directly perceived, using HP-3260B test experiments example 1 and the power-up properties of flow of comparative example.
As shown in Fig. 2 for powering up properties of flow comparison diagram, in figure, longitudinal axis △ L/L represent the inductance value rate of change of compound soft magnetic material magnet ring,
The power-up properties of flow of experimental example 1 is substantially better than comparative example as we know from the figure, can also show that experimental example 1 is relative from power-up properties of flow
There is high Bs in comparative example.This is possibly due to：FeSiCr alloys with the saturation induction density higher than NiCuZn, with
The important original that FeSiCr alloys are significantly lifted relative to comparative example as the power-up properties of flow that main material is probably experimental example 1
Therefore one.
Above content is with reference to specific 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 general technical staff of the technical field of the invention,
Some replacements or obvious modification is made on the premise of without departing from present inventive concept, and performance or purposes are identical, should all be considered as
Belong to protection scope of the present invention.
Claims (10)
1. a kind of compound soft magnetic material, it is characterised in that：Material includes the component of following percentage by weight：75.13～
The FeSiCr alloy powders of 86.12wt%, the Fe of 9～14.5wt%2O3, 1.95～2.99wt% NiO, 2.15～
The ZnO of 3.75wt%, the CuO of 0.55～1.43wt%, the Bi of 0.03～0.85wt%2O3, 0.15～0.45wt% V2O5、
The SiO of 0.05～0.9wt%2；The compound soft magnetic material by said components mixing after, Jing pre-burnings, crushing, pelletize, compacting and
It is obtained after sintering.
2. compound soft magnetic material according to claim 1, it is characterised in that：The mean diameter of the FeSiCr alloy powders
For 3～30 μm, remaining component is nano material, and particle diameter is 50～100nm.
3. compound soft magnetic material according to claim 1, it is characterised in that：Count by weight percentage, the FeSiCr
The content of alloy powder is 82.1wt%, and the content of the Fe2O3 is 10.3wt%, and the content of the NiO is 2.5wt%, institute
The content for stating ZnO is 3.1wt%, and the content of the CuO is 0.9wt%, and the content of the Bi2O3 is 0.5wt%, the V2O5
Content be 0.25wt%, the content of the SiO2 is 0.35wt%.
4. a kind of manufacture method of compound soft magnetic material, it is characterised in that：According to the component proportion dispensing of following percentage by weight：
The FeSiCr alloy powders of 75.13～86.12wt%, the Fe of 9～14.5wt%2O3, 1.95～2.99wt% NiO, 2.15～
The ZnO of 3.75wt%, the CuO of 0.55～1.43wt%, the Bi of 0.03～0.85wt%2O3, 0.15～0.45wt% V2O5、
The SiO of 0.05～0.9wt%2；By the dispensing after mixing, pre-burning, crushing, pelletize, compacting and sintering, it is obtained described multiple
Close soft magnetic materials.
5. the manufacture method of compound soft magnetic material according to claim 4, it is characterised in that：Specifically include following steps：
1) mix：The good dispensing of proportioning is carried out into dry mixed, incorporation time is 60～90 minutes；
2) pre-burning：The material for mixing is carried out into pre-burning under nitrogen protection atmosphere and obtains Preburning material, calcined temperature is controlled 700
± 20 DEG C, burn-in time is 200～300 minutes, and during pre-burning, Control for Oxygen Content is below 1%；
3) crush：By the step 2) Preburning material that obtains carries out waterproof pulverization, with dehydrated alcohol as solvent during crushing, during crushing
Between be 60～120 minutes, after crushing control slip particle diameter at 3～30 μm；
4) pelletize：In the slip, add the resin for dissolving in dehydrated alcohol equivalent to the 3～4% of the slip weight to glue
Knot agent, protects mist projection granulating using nitrogen, obtains particulate material；
5) suppress：Blank is obtained by the particulate material compressing, the pressed density of the blank is controlled in (5.55 ± 0.10)
g/cm3；
6) sinter：The blank is sintered under nitrogen protection atmosphere, sintering temperature is controlled at 750 DEG C～790 DEG C, sintering
When Control for Oxygen Content below 1%；200～300 minutes are incubated after sintering, room temperature is then cooled to, the composite soft-magnetic is obtained
Material.
6. the manufacture method of compound soft magnetic material according to claim 5, it is characterised in that：The step 2) in push pedal
Pre-burning is carried out in kiln.
7. the manufacture method of compound soft magnetic material according to claim 5, it is characterised in that：The step 4) middle addition phase
When in the slurry weight 3.5% the resinoid bond for dissolving in dehydrated alcohol.
8. the manufacture method of compound soft magnetic material according to claim 5, it is characterised in that：The step 4) described in can
The resinoid bond for being dissolved in dehydrated alcohol is furfural resin.
9. the manufacture method of compound soft magnetic material according to claim 5, it is characterised in that：The step 5) in adopt powder
Last forming machine obtains blank by the particulate material compressing.
10. the manufacture method of compound soft magnetic material according to claim 5, it is characterised in that：The step 6) in electricity
It is sintered in resistance stove.
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| CN105177396A (en) * | 2015-09-01 | 2015-12-23 | 深圳顺络电子股份有限公司 | Iron alloy composite and preparation method thereof |
| WO2017193384A1 (en) | 2016-05-13 | 2017-11-16 | 深圳顺络电子股份有限公司 | Soft magnetic composite material and manufacturing method thereof |
| CN107275033B (en) * | 2017-05-23 | 2019-01-08 | 深圳顺络电子股份有限公司 | A kind of magnetically soft alloy material and preparation method thereof |
| CN111446056A (en) * | 2020-03-31 | 2020-07-24 | 江苏普隆磁电有限公司 | Soft magnetic powder material |
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