CN108597717A - The preparation method of nucleocapsid soft-magnetic composite material - Google Patents
The preparation method of nucleocapsid soft-magnetic composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 73
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 18
- 239000000956 alloy Substances 0.000 claims abstract description 18
- 239000002184 metal Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000006247 magnetic powder Substances 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000012266 salt solution Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011701 zinc Substances 0.000 claims abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 230000001376 precipitating effect Effects 0.000 claims abstract description 10
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 claims abstract description 7
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 claims abstract description 7
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 5
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 30
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- LXJXRIRHZLFYRP-VKHMYHEASA-N D-glyceraldehyde 3-phosphate Chemical compound O=C[C@H](O)COP(O)(O)=O LXJXRIRHZLFYRP-VKHMYHEASA-N 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- 238000002161 passivation Methods 0.000 claims description 12
- 238000011282 treatment Methods 0.000 claims description 10
- 229910000859 α-Fe Inorganic materials 0.000 claims description 10
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 239000011572 manganese Substances 0.000 claims description 4
- 238000000643 oven drying Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 229910017060 Fe Cr Inorganic materials 0.000 claims description 3
- 229910002544 Fe-Cr Inorganic materials 0.000 claims description 3
- 229910017082 Fe-Si Inorganic materials 0.000 claims description 3
- 229910017133 Fe—Si Inorganic materials 0.000 claims description 3
- 229910003296 Ni-Mo Inorganic materials 0.000 claims description 3
- 229910002796 Si–Al Inorganic materials 0.000 claims description 3
- 229910008458 Si—Cr Inorganic materials 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 229910001004 magnetic alloy Inorganic materials 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 244000025254 Cannabis sativa Species 0.000 claims 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000011162 core material Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000005253 cladding Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000006698 induction Effects 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 239000011257 shell material Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 229910002555 FeNi Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical group [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 241000549556 Nanos Species 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydrogen Sodium hydroxide Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 210000000329 smooth muscle myocyte Anatomy 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/33—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials mixtures of metallic and non-metallic particles; metallic particles having oxide skin
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Soft Magnetic Materials (AREA)
Abstract
This application discloses a kind of preparation methods of nucleocapsid soft-magnetic composite material, in turn include the following steps：S1 prepares quantitative magnetic metallic powder；S2 determines the corresponding molal weight of required metallic element Mn or Ni, Fe, Zn according to required manganese-zinc ferrite or nickel-zinc ferrite covering amount, configures the metal salt solution of the corresponding molal weight；Deionized water is added in magnetic metallic powder and stirs in step 1 by S3, is heated to 30 80 DEG C；S4 is slowly dropped into metal salt solution described in step S2, while stirring and instilling simultaneously precipitating reagent, and control pH reacts 30 60min, obtain alloy magnetic powder 9 11；S5 is dried after cleaning above-mentioned alloy magnetic powder；Alloy magnetic powder after drying is sintered 1 3h by S6 at a temperature of 500 700 DEG C, obtains nucleocapsid particles；Above-mentioned nucleocapsid particles at room temperature to be pressed into magnetic core under the pressure of 1400Mpa, are then sintered 1 hour at 600 DEG C and obtain nucleocapsid soft-magnetic composite material by S7.The nucleocapsid soft-magnetic composite material that the present invention prepares is had excellent performance.
Description
Technical field
This application involves soft magnetic property material and powder metallurgical technology, more particularly to a kind of nucleocapsid soft-magnetic composite material
Preparation method.
Background technology
With the fast development of microelectric technique and magnetic electron device, the development of the core material with excellent magnetic energy is
As the field one of critical issue urgently to be resolved hurrily.Soft magnetic materials is widely used in transformer, motor and instrument and equipment neck
Domain.In various magnetic materials, metal material is with the low characteristic of saturation induction density and magnetic conductivity height, power attenuation.But
The high frequency eddy current losses of metal material are higher, limit its application in high frequency field.In contrast, though ferrite is saturated magnetic strength
Answer intensity relatively low, but since it with high resistivity can be used for higher frequency.By insulating in metal material surface
Cladding can block effective contact between powder particle, increase the sample resistivity after composite molding.Frequency applications when
It waits, this layer of cladding insulating film can significantly reduce the energy loss that the vortex phenomenon of material is brought, so as to improve the high frequency of material
Performance.When low frequency applications, although the effect of cladding insulating film is without so obviously, can also reduce the damage that vortex phenomenon is brought
Consumption.Therefore, soft-magnetic composite material made of the magnetic-particle of insulating wrapped（Soft Magnetic Composites, SMCs）,
Due to good thermal stability, high magnetic permeability and low eddy-current loss, causing sizable concern.
So far, researcher has used a variety of methods oxide coated on alloying pellet, as sol-gal process,
Legal, coprecipitation of hydro-thermal etc. reduces loss to improve resistivity.Surrounding phase common at present includes SiO2、Al2O3、MgO、
NiO etc., but there are some disadvantages for these surrounding phases, and prepared soft-magnetic composite material surrounding phase content is low will to be not enough to inhibit whirlpool
Stream loss.And these surrounding phases are all non-magnetic phases, and in the presence of a large amount of surrounding phase, meeting diluted magnetic energy reduces full
With magnetic induction intensity and magnetic conductivity.Therefore, magnetic of the nucleocapsidization with high saturated magnetic induction and stability is prepared
Grain is very important.Ferrite has many advantages, such as that resistivity is high, loss is low, high frequency characteristics is good and is used as shell material, by
It is widely used in the covering material of metal and alloy powder particle.Schonlein M et al. synthesize Fe/iron using traditional ceramics method
The shell-nuclear compounded material of oxysome shows that the core loss of composite material is less than 250 Ω/H, is less than original core loss（800Ω/
H）, there is high magnetic conductivity stability.Other scholars coat ferrite using different methods in metal and alloy powder surface,
As a result it confirms that ferrite is covered by iron core, can significantly improve resistivity, reduces loss, especially improved in high-frequency
The stability of magnetic conductivity.
Directly mixing between alloy powder and ferrite powder is difficult to be formed complete cladding, affects covered effect,
And then affect the reduction of magnetic loss, therefore magnetic powder core loss further decreases, and needs ferrite covering evenly, to make
Be completely coated on alloy powder surface.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of nucleocapsid soft-magnetic composite material, by changing metal magnetic powder
Last surface tension improves ferrite soft magnetic covered effect, avoids the occurrence of hollow powder, satellite powder, bonded powder, increase the cause of clad
It is easily controllable, narrow particle size distribution to prepare sphericity height, any surface finish, particle size to improve the performance of magnetic powder for close property
Nucleocapsid particles；Obtained nucleocapsid soft-magnetic composite material density is not less than 7.2g cm-3, and by 700 DEG C and 900 DEG C
After heat treatment, density does not have larger change；The ferritic toroidal core containing 5wt% shows excellent soft magnet performance, magnetic
Conductance is 56, and saturation magnetization is 127.1emu/g, and core loss is about 1.51w/kg at 100kHz and 50mT.
To achieve the above object, the present invention provides the following technical solutions：
The embodiment of the present application discloses a kind of preparation method of nucleocapsid soft-magnetic composite material, in turn includes the following steps：
S1 prepares quantitative magnetic metallic powder；
S2 according to required manganese-zinc ferrite or nickel-zinc ferrite covering amount determine needed for metallic element Mn or Ni, Fe, Zn it is corresponding
Molal weight configures the metal salt solution of the corresponding molal weight；
Deionized water is added in magnetic metallic powder and stirs in step 1 by S3, is heated to 30-80 DEG C；
S4 is slowly dropped into metal salt solution described in step S2, while stirring and instilling simultaneously precipitating reagent, control pH in 9-11,
30-60min is reacted, alloy magnetic powder is obtained；
S5 is dried after cleaning above-mentioned alloy magnetic powder；
Alloy magnetic powder after drying is sintered 1-3h by S6 at a temperature of 500-700 DEG C, obtains nucleocapsid particles；
S7 under the pressure of 1400Mpa by above-mentioned nucleocapsid particles at room temperature to be pressed into magnetic core, and then sintering 1 is small at 600 DEG C
When obtain nucleocapsid soft-magnetic composite material.
Preferably, in the preparation method of above-mentioned nucleocapsid soft-magnetic composite material, the magnetic metallic powder be pure Fe powder,
Fe-Si powder, Fe-Al powder, Fe-Cr powder, Fe-Si-Al powder, Fe-Si-Cr powder, Fe-Ni powder, Fe-Ni-Mo powder, Fe base amorphous nanos
It is one or more in brilliant soft-magnetic alloy powder, 50 μm of the magnetic metallic powder grain size ＜.
Preferably, in the preparation method of above-mentioned nucleocapsid soft-magnetic composite material, the metal salt solution is villaumite, nitric acid
It is one or more in salt, sulfate, carbonate.
Preferably, in the preparation method of above-mentioned nucleocapsid soft-magnetic composite material, the precipitating reagent is ammonium oxalate solution or hydrogen
Sodium hydroxide solution, the precipitant concentration are 1-2mol/L.
Preferably, in the preparation method of above-mentioned nucleocapsid soft-magnetic composite material, the covering amount is manganese-zinc ferrite or nickel
The mass ratio of Zn ferrite and magnetic metallic powder, the covering amount ＜ 10%.
Preferably, in the preparation method of above-mentioned nucleocapsid soft-magnetic composite material, the magnetic metal powder before the step S3
End first carries out Passivation Treatment, and the Passivation Treatment includes the following steps：
1）Passivator is configured, the passivator includes triosephosphate solution, sulfuric acid solution and phosphoric acid solution, and the triosephosphate is molten
The mass fraction of triosephosphate is 2%-10% in liquid, and the mass fraction of sulfuric acid is 2%-10%, the phosphoric acid in the sulfuric acid solution
The mass fraction of phosphoric acid is 2%-10% in solution.
2）Passivation reaction the magnetic metallic powder is added in above-mentioned passivator, uniform stirring, after 15min, spend from
Sub- water is washed 3-4 times, then puts vacuum drying oven drying into.
Preferably, in the preparation method of above-mentioned nucleocapsid soft-magnetic composite material, each metal ion of metal salt solution
Molal weight ratio is Fe3+∶Zn2+∶Mn2+Or Ni2+=2∶（1-x）: x, wherein 0 ＜ x ＜ 1.
Preferably, in the preparation method of above-mentioned nucleocapsid soft-magnetic composite material, in step S5 using deionized water cleaning or
Person, which is placed in ethyl alcohol, uses ultrasonic cleaning, and drying temperature is 80-100 DEG C in step S5.
Preferably, in the preparation method of above-mentioned nucleocapsid soft-magnetic composite material, stir speed (S.S.) point in step S3 and step S4
It Wei not 200r/min.
Preferably, in the preparation method of above-mentioned nucleocapsid soft-magnetic composite material, the instillation rate of precipitating reagent is in step S4
5ml/min。
Magnetic metallic powder may be used china-clay method, chemical coprecipitation, hydro-thermal method, mechanical attrition method, sol-gal process,
Prepared by any one of Sol-Gel-Self-Propagating Process, spray drying process method, be preferably prepared into spherical powder.
On the one hand the Passivation Treatment of magnetic metallic powder makes magnetic metallic powder particle mutually insulated, and then can reach drop
Low-loss improves the purpose of quality factor, is on the other hand ensureing the best situation of magnetic metallic powder core insulation covered effect
Under, the insulating layer coated between magnetic metallic powder should get over Bao Yuehao, and powder can be made in high temperature compacting and subsequent heat treatment work
Skill promotes to bond, and reaches the consistency and mechanical strength purpose for improving powder core.The result shows that Passivation Treatment can be substantially reduced
The loss of soft magnetic-powder core.The effect of passivator mainly improves the adhesive force of paint film（It is to improve ferrite in alloy surface herein
Adhesive force）, while protecting metals against corrosion（Traditional non magnetic shell compactness is inadequate, and corrosive substance can be caused saturating
It crosses shell and enters stratum nucleare and alloyed powder is corroded）.
Specific implementation mode
The technical program is illustrated below in conjunction with embodiment.
Embodiment 1
1）Manganese-zinc ferrite, covering amount, the i.e. mass ratio of the quality of manganese-zinc ferrite and magnetic metallic powder are selected in early-stage preparations
It is set as 5%, molal weight ratio Fe: Zn: Mn=2 of metallic element in manganese-zinc ferrite:0.5:0.5, prepare phase by above-mentioned requirements
The magnetic metallic powder of quality is answered, and configures the chloride solution of Fe, Zn, Mn containing corresponding molal weight, magnetic metallic powder
Using Fe-Ni powder, grain size is 40-50 μm.
2）Passivation Treatment：Fe-Ni powder is added in passivator, uniform stirring, after 15min, is washed 4 times with deionized water,
Then vacuum drying oven drying is put into, passivator includes triosephosphate solution, sulfuric acid solution and phosphoric acid solution, triosephosphate solution
The mass fraction of middle triosephosphate is 4%, and the mass fraction of sulfuric acid is 2% in sulfuric acid solution, the quality point of phosphoric acid in phosphoric acid solution
Number is 3%.
3）Deionized water is added in Fe-Ni powder after Passivation Treatment and is stirred, control stir speed (S.S.) is 200r/min, heating
To 60 DEG C, it is slowly dropped into chloride solution, while stirring and instilling simultaneously precipitating reagent, control stir speed (S.S.) is 200r/min, precipitation
The instillation rate of agent is 5ml/min, and control pH reacts 60min 10 or so, obtains alloy magnetic powder, and precipitating reagent uses hydroxide
Sodium solution, precipitant concentration 2mol/L.
4）It dries at a temperature of 80 DEG C after alloy magnetic powder is cleaned up using deionized water, is burnt at a temperature of 700 DEG C after drying
3h is tied, FeNi/Mn is obtained0.5Zn0.5Fe2O4Nucleocapsid particles, at room temperature to be pressed into toroidal core under the pressure of 1400Mpa,
Then it is sintered 1 hour at 600 DEG C and obtains nucleocapsid soft-magnetic composite material.
Embodiment 2
1）Nickel-zinc ferrite, covering amount, the i.e. mass ratio of the quality of nickel-zinc ferrite and magnetic metallic powder are selected in early-stage preparations
It is set as 5%, molal weight ratio Fe: Zn: Ni=2 of metallic element in nickel-zinc ferrite:0.4:0.6, prepare phase by above-mentioned requirements
The magnetic metallic powder of quality is answered, and configures the sulfate liquor of Fe, Zn, Ni containing corresponding molal weight, magnetic metal powder
It is 40-50 μm that end, which uses Fe-Ni powder, grain size,.
2）Passivation Treatment：Fe-Ni powder is added in passivator, uniform stirring, after 15min, is washed 4 times with deionized water,
Then vacuum drying oven drying is put into, passivator includes triosephosphate solution, sulfuric acid solution and phosphoric acid solution, triosephosphate solution
The mass fraction of middle triosephosphate is 3%, and the mass fraction of sulfuric acid is 2% in sulfuric acid solution, the quality point of phosphoric acid in phosphoric acid solution
Number is 4%.
3）Deionized water is added in Fe-Ni powder after Passivation Treatment and is stirred, control stir speed (S.S.) is 200r/min, heating
To 80 DEG C, it is slowly dropped into sulfate liquor, while stirring and instilling simultaneously precipitating reagent, control stir speed (S.S.) is 200r/min, is sunk
The instillation rate of shallow lake agent is 5ml/min, and control pH reacts 60min 10 or so, obtains alloy magnetic powder, and precipitating reagent uses oxalic acid
Ammonium salt solution, precipitant concentration 1.8mol/L.
4）By alloy magnetic powder be placed in ethyl alcohol with ultrasonic cleaning it is clean after dry at a temperature of 90 DEG C, 700 DEG C of temperature after drying
Degree is lower to be sintered 2.8h, obtains FeNi/Ni 0.6Zn0.4Fe2O4Nucleocapsid particles, at room temperature to be pressed under the pressure of 1400Mpa
Then toroidal core is sintered 1 hour at 600 DEG C and obtains nucleocapsid soft-magnetic composite material.
The density for the nucleocapsid soft-magnetic composite material that detection embodiment 1-2 is obtained, and detection is by 700 DEG C and 900 DEG C
Density after heat treatment, as a result such as following table（Unit g cm-3）：
| Embodiment | Density | Density after 700 DEG C of heat treatments | Density after 900 DEG C of heat treatments |
| Embodiment 1 | 7.32 | 7.31 | 7.30 |
| Embodiment 2 | 7.25 | 7.24 | 7.24 |
The soft magnet performance of embodiment 1-2 is detected, as a result such as following table：
| Embodiment | Magnetic conductivity | Saturation magnetization（emu / g） | Core loss under 100kHz and 50mT（w / kg） |
| Embodiment 1 | 56 | 127.1 | 1.51 |
| Embodiment 2 | 57 | 127.2 | 1.50 |
It should be noted that above-described embodiment does not only limit its protection domain to the exemplary illustration of this patent, this
Field personnel can also carry out local change to it, as long as it does not exceed the essence of this patent, all be considered as to this patent
Equivalent replacement, all within the protection domain of this patent, such as：Magnetic metallic powder be pure Fe powder, Fe-Si powder, Fe-Al powder,
In Fe-Cr powder, Fe-Si-Al powder, Fe-Si-Cr powder, Fe-Ni powder, Fe-Ni-Mo powder, Fe based amorphous nano soft-magnetic alloy powders
One or more, 50 μm of magnetic metallic powder grain size ＜；Metal salt solution is in villaumite, nitrate, sulfate, carbonate
It is one or more.
Claims (10)
1. a kind of preparation method of nucleocapsid soft-magnetic composite material, which is characterized in that in turn include the following steps：
S1 prepares quantitative magnetic metallic powder；
S2 according to required manganese-zinc ferrite or nickel-zinc ferrite covering amount determine needed for metallic element Mn or Ni, Fe, Zn it is corresponding
Molal weight configures the metal salt solution of the corresponding molal weight；
Deionized water is added in magnetic metallic powder and stirs in step 1 by S3, is heated to 30-80 DEG C；
S4 is slowly dropped into metal salt solution described in step S2, while stirring and instilling simultaneously precipitating reagent, control pH in 9-11,
30-60min is reacted, alloy magnetic powder is obtained；
S5 is dried after cleaning above-mentioned alloy magnetic powder；
Alloy magnetic powder after drying is sintered 1-3h by S6 at a temperature of 500-700 DEG C, obtains nucleocapsid particles；
S7 under the pressure of 1400Mpa by above-mentioned nucleocapsid particles at room temperature to be pressed into magnetic core, and then sintering 1 is small at 600 DEG C
When obtain nucleocapsid soft-magnetic composite material.
2. the preparation method of nucleocapsid soft-magnetic composite material according to claim 1, which is characterized in that the magnetic metal powder
End be pure Fe powder, Fe-Si powder, Fe-Al powder, Fe-Cr powder, Fe-Si-Al powder, Fe-Si-Cr powder, Fe-Ni powder, Fe-Ni-Mo powder,
It is one or more in Fe based amorphous nano soft-magnetic alloy powders, 50 μm of the magnetic metallic powder grain size ＜.
3. the preparation method of nucleocapsid soft-magnetic composite material according to claim 1, which is characterized in that the metal salt solution
It is one or more in villaumite, nitrate, sulfate, carbonate.
4. the preparation method of nucleocapsid soft-magnetic composite material according to claim 1, which is characterized in that the precipitating reagent is grass
Acid ammonium solution or sodium hydroxide solution, the precipitant concentration are 1-2mol/L.
5. the preparation method of nucleocapsid soft-magnetic composite material according to claim 1, which is characterized in that the covering amount is manganese
The mass ratio of Zn ferrite or nickel-zinc ferrite and magnetic metallic powder, the covering amount ＜ 10%.
6. the preparation method of nucleocapsid soft-magnetic composite material according to claim 1, which is characterized in that before the step S3
The magnetic metallic powder first carries out Passivation Treatment, and the Passivation Treatment includes the following steps：
1）Passivator is configured, the passivator includes triosephosphate solution, sulfuric acid solution and phosphoric acid solution, and the triosephosphate is molten
The mass fraction of triosephosphate is 2%-10% in liquid, and the mass fraction of sulfuric acid is 2%-10%, the phosphoric acid in the sulfuric acid solution
The mass fraction of phosphoric acid is 2%-10% in solution；
2）Passivation reaction the magnetic metallic powder is added in above-mentioned passivator, uniform stirring, after 15min, uses deionized water
Then vacuum drying oven drying is put in washing 3-4 times into.
7. the preparation method of nucleocapsid soft-magnetic composite material according to claim 1, which is characterized in that the metal salt solution
The molal weight ratio of each metal ion is Fe3+∶Zn2+∶Mn2+Or Ni2+=2∶（1-x）: x, wherein 0 ＜ x ＜ 1.
8. the preparation method of nucleocapsid soft-magnetic composite material according to claim 1, which is characterized in that use and go in step S5
Ionized water, which is cleaned or is placed in ethyl alcohol, uses ultrasonic cleaning, and drying temperature is 80-100 DEG C in step S5.
9. the preparation method of nucleocapsid soft-magnetic composite material according to claim 1, which is characterized in that step S3 and step S4
Middle stir speed (S.S.) is respectively 200r/min.
10. the preparation method of nucleocapsid soft-magnetic composite material according to claim 1, which is characterized in that precipitated in step S4
The instillation rate of agent is 5ml/min.
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