CN106006751A - Preparation method of cobalt-doped nickel zinc ferrite nanometer materials - Google Patents
Preparation method of cobalt-doped nickel zinc ferrite nanometer materials Download PDFInfo
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Abstract
A preparation method of cobalt-doped nickel zinc ferrite nanometer materials comprises the steps that 1, on the basis of the stoichiometric ratio of NixZnyCo(1-x-y)Fe2O4, nickel nitrate, zinc nitrate, cobalt nitrate and ferric nitrate are weighed, wherein 0.75<=x+y<=0.95, 0.4<=x<=0.6, and 0.15<=y<=0.4; the raw materials are dissolved into distilled water, and a surface active agent is added to obtain a red brown mixed solution; 2, uniform stirring is performed in thermostatic water, a sodium hydroxide solution is added dropwise, pH of the mixed solution is adjusted to 9-12, and a reaction precursor is obtained; 3, normal temperature aging is performed, and a thick aging solution is obtained; 4, a crystallization solution is obtained after crystallization; 5, vacuumizing is performed to obtain filter cakes; 6, drying is performed, and then grinding is performed to obtain cobalt-doped nickel zinc ferrite nanometer materials. According to the cobalt-doped nickel zinc ferrite nanometer materials, particles are spherical, the average grain diameter is 20-30 nanometers, the high magnetic conductivity and low dielectric constant are obtained under the wave band being 2-4 GHz, the defect that a traditional ferrite is poor in wave absorption effect within the low-frequency S-wave band range is overcome, and the wave absorption performance of the ferrite is improved.
Description
Technical field
The invention belongs to magnetic Nano material and manufacture field, particularly to the preparation of the Ni-Zn ferrite nano materials of a kind of cation doping
Method.
Background technology
Nanometer spinel type nickel-zinc ferrite has dielectric loss and magnetic hystersis loss double grading, its high resistance as absorbing material
The attributes such as rate, high magnetic permeability, low-dielectric loss, high-curie temperature and chemical stability, inhale wave technology field in many and play pass
Key effect.It is mainly used in manufacture on and off switch, transformator, loading coil, radar equipment, stealth material, electronics and micro-
Wave device.But owing to single ferrite is difficult to meet absorption band width, light weight, requirement that thickness is thin, therefore at ferrite
Adulterate in micropowder some additives composition composite absorber, it is achieved controlled to microwave absorption intensity, bandwidth and electromagnetic parameter
Regulation.
Traditional dry method doping is difficult to control due to doping, it is difficult to uniformly mixes, is readily incorporated other impurity；And wet method doping
Avoid the defect of Traditional dopant method, make alloy and ferrite mix homogeneously on atom or molecular scale, can accurately control
Doping processed, is effectively improved the performance of nickel-zinc ferrite.
The existing method preparing nanometer ferrite mainly has: chemical coprecipitation, low-temperature solid phase reaction precursor process, self-propagating
Combustion synthesis method, sol-gel process etc..But traditional synthetic method craft is complicated, environmental requirement is harsh and cost is the highest, unfavorable
In industrialized production.The present invention uses hydrothermal synthesis method, in high temperature, high-pressure sealed environment, adopts and uses water as reaction media,
Add surfactant before the synthesis and promote to generate the surface energy of uniform precursors, reduction crystal, make indissoluble or insoluble matter
Matter dehydration is dissolved, and carries out recrystallization.The nanoparticle crystal grain utilizing hydrothermal synthesis method to prepare is tiny, and defect is few, well-crystallized,
Lattice is grown completely, and particle diameter narrow distribution, reunion degree is low.Preparation process need not high temperature sintering, it is to avoid crystal grain reunion,
Grow up, the formation of defect.The method is simple, low cost, reaction condition gentleness are easily controlled.
At present, ferrite wave-absorbing material production cost is the highest, is unfavorable for that commercial introduction, in daily life, is inhaled ripple scope and mainly concentrated
In 8-18GHz frequency band, bad at the absorbing property of low frequency S-band (2-4GHz), and the main source of electromagenetic wave radiation it
In the range of one wireless propagation concentrates on 2-6GHz.Along with electromagnetic radiation situation increasingly serious in life, prepare cost
Low, technique simply and has important value at the ferrite that electromagnetic wave low frequency S-band (2-4GHz) absorbing property is good.
Summary of the invention
For the deficiencies in the prior art, the invention provides the preparation method of the Ni-Zn ferrite nano materials of a kind of cation doping, real
Show the ferrite absorbing property at low-frequency band, be that a kind of method is simple, low cost, reaction condition are easily-controllable, environmental protection and energy saving,
Preparation method at the Ni-Zn ferrite nano materials of the good cation doping of low frequency S-band (2-4GHz) absorbing property.
The preparation method of the Ni-Zn ferrite nano materials of the cation doping of the present invention, comprises the following steps:
Step 1, dispensing:
(1) Ni is pressedxZnyCo(1-x-y)Fe2O4Stoichiometric proportion, weighs 4 kinds of raw materials respectively: nickel nitrate (Ni (NO3)2·6H2O)、
Zinc nitrate (Zn (NO3)2·6H2O), cobalt nitrate (Co (NO3)2·6H2And ferric nitrate (Fe (NO O)3)3·9H2O), wherein, 0.75
≤ x+y≤0.95,0.4≤x≤0.6,0.15≤y≤0.4；
(2) by above-mentioned 4 kinds of raw materials, it is dissolved in distilled water, adds surfactant, after being uniformly dispersed, obtain russet
Mixed solution；Wherein, in mass ratio, 4 kinds of raw materials quality and: distilled water=(25～28): (150～200), 4 kinds of raw materials quality
With: surfactant=(25～28): (1～3)；
Step 2: reaction of formation presoma；
Mixed solution russet is placed in four-hole boiling flask, water bath with thermostatic control 30～50 DEG C, continues with 150～270r/min rotating speeds
Uniform stirring；In four-hole boiling flask, drip the sodium hydroxide solution of 1～3mol/L, the pH=9～12 of regulation mixed solution simultaneously；
Step 3, ageing:
By precursors, in the static ageing of room temperature 6～10h, remove section top clear liquid, obtain lower floor's thick ageing liquid；
Step 4, crystallization:
(1) by thick for lower floor ageing liquid, concussion shakes up, and moves into teflon-lined hydro-thermal autoclave；
(2) by hydro-thermal autoclave, at 160～220 DEG C, crystallization 6～12h, obtain crystallization liquid；
Step 5, sucking filtration:
Crystallization liquid is cooled to room temperature, and the solution washing obtained, to neutrality, vacuum filtration, obtains filter cake；
Step 6, dries and grinds:
(1) by filter cake 60～80 DEG C of drying, pitchy block is obtained；
(2) pitchy block is ground to powder body, i.e. obtains the Ni-Zn ferrite nano materials of cation doping.
In described step 1 (1), nickel nitrate, zinc nitrate, cobalt nitrate and ferric nitrate are analytical pure.
In described step 1 (2), surfactant is Polyethylene Glycol.
In described step 1 (2), supersound process is used to make it be uniformly dispersed.
In described step 2 (2), the speed of dropping sodium hydroxide solution is 0.5～1 drop/sec.
In described step 4 (2), crystallization is carried out in cabinet-type electric furnace.
In described step 5, use distilled water and absolute ethanol washing.
In described step 6 (1), air dry oven is used to dry.
The preparation method of the Ni-Zn ferrite nano materials of the cation doping of the present invention, compared with prior art, advantages of the present invention exists
In:
The ferrite of the present invention is the Spinel nickel zinc cobalt ferrites of pure phase, and sample particle is that class is spherical, and mean diameter is about
20～30nm, at 2-4GHz wave band, there is higher pcrmeability and relatively low dielectric constant, compensate for conventional iron oxysome at low frequency S
The defect that in wavelength band, wave-absorbing effect is the best, improves ferritic absorbing property.On the basis of using hydrothermal synthesis method,
By the electromagnetic parameter of doping Co unit usually controlled material self, reach to improve the purpose of material electromagnetic performance；At temperate condition
Under, utilize water miscible inorganic metal salt for raw material, reduce cost；Stoichiometrically the slaine of doping is dissolved directly into
In reactant solution, can accurately control doping, it is to avoid introduce other impurity；During crystallization, anti-by controlling
Answer temperature and time, regulate and control ferritic crystal formation and crystallite dimension, thus synthesize the nano nickel zinc ferro-cobalt oxygen that electromagnetic performance is good
Body.Preparation method is simple, low cost, and reaction condition is easily-controllable, environmental protection and energy saving, and product particle size is tiny, and defect is few, crystallizes good
Good, reunion degree is low, it is adaptable to industrialized production.
Accompanying drawing explanation
The process chart of the preparation method of the Ni-Zn ferrite nano materials of the cation doping of Fig. 1 embodiment of the present invention；
The scanning electron microscopic picture of the Ni-Zn ferrite nano materials of the cation doping of Fig. 2 embodiment of the present invention 1 preparation；
The scanning electron microscopic picture of the Ni-Zn ferrite nano materials of the cation doping of Fig. 3 embodiment of the present invention 2 preparation；
The scanning electron microscopic picture of the Ni-Zn ferrite nano materials of the cation doping of Fig. 4 embodiment of the present invention 3 preparation；
The scanning electron microscopic picture of the Ni-Zn ferrite nano materials of the cation doping of Fig. 5 embodiment of the present invention 4 preparation；
The scanning electron microscopic picture of the Ni-Zn ferrite nano materials of the cation doping of Fig. 6 embodiment of the present invention 5 preparation；
The scanning electron microscopic picture of the Ni-Zn ferrite nano materials of the cation doping of Fig. 7 embodiment of the present invention 6 preparation；
The scanning electron microscopic picture of the Ni-Zn ferrite nano materials of the cation doping of Fig. 8 embodiment of the present invention 7 preparation；
The scanning electron microscopic picture of the Ni-Zn ferrite nano materials of the cation doping of Fig. 9 embodiment of the present invention 8 preparation.
Detailed description of the invention
The process chart of the preparation method of the Ni-Zn ferrite nano materials of the cation doping of following example is shown in Fig. 1.
Embodiment 1
The preparation method of the Ni-Zn ferrite nano materials of a kind of cation doping, comprises the following steps:
Step 1, dispensing:
(1) Ni is pressed0.5Zn0.4Co0.1Fe2O4Stoichiometric proportion, weighs 4 kinds of raw materials respectively: 3.64g analytical pure nickel nitrate
(Ni(NO3)2·6H2O), 2.97g analytical pure zinc nitrate (Zn (NO3)2·6H2O), 0.73g analytical pure cobalt nitrate
(Co(NO3)2·6H2And 20.20g analytical pure ferric nitrate (Fe (NO O)3)3·9H2O)；
(2) by above-mentioned 4 kinds of raw materials, being dissolved in 150mL distilled water, add 2g Polyethylene Glycol, supersound process makes it disperse
Uniformly, mixed solution russet is obtained；
Step 2: reaction of formation presoma；
Mixed solution russet is placed in four-hole boiling flask, water bath with thermostatic control 30 DEG C, stirs with 210r/min rotating speed continuous uniform；
In four-hole boiling flask, drip the sodium hydroxide solution of 3mol/L, the pH=11 of regulation mixed solution simultaneously；
Step 3, ageing:
By precursors, at room temperature static ageing 10h, remove section top clear liquid, obtain lower floor's thick ageing liquid；
Step 4, crystallization:
(1) by thick for lower floor ageing liquid, concussion shakes up, and moves into teflon-lined hydro-thermal autoclave；
(2) by hydro-thermal autoclave, in the cabinet-type electric furnace of 160 DEG C, crystallization 6h, obtain crystallization liquid；
Step 5, sucking filtration:
Crystallization liquid is cooled to room temperature, respectively washs 4 times with distilled water and dehydrated alcohol, make solution the most neutral, vacuum filtration,
Obtain filter cake；
Step 6, dries and grinds:
(1) filter cake is dried in the drying baker of 60 DEG C, obtain pitchy block；
(2) pitchy block is ground to powder body, i.e. obtains the Ni-Zn ferrite nano materials of cation doping.
Ni prepared by the present embodiment0.5Zn0.4Co0.1Fe2O4The Ni-Zn ferrite nano materials of cation doping, scanning electron microscopic picture is shown in accompanying drawing
2, its mean diameter is 20-30nm, and this nickel zinc cobalt ferrites is 3.1 at the pcrmeability real part of 3GHz Frequency point, and imaginary part is 3.0；
Real part of permittivity is 7.2, and imaginary part is 0.16.
Embodiment 2
The preparation method of the Ni-Zn ferrite nano materials of a kind of cation doping, comprises the following steps:
Step 1, dispensing:
(1) Ni is pressed0.6Zn0.15Co0.25Fe2O4Stoichiometric proportion, weighs 4 kinds of raw materials respectively: 4.36g analytical pure nickel nitrate
(Ni(NO3)2·6H2O), 1.12g analytical pure zinc nitrate (Zn (NO3)2·6H2O), 1.82g analytical pure cobalt nitrate
(Co(NO3)2·6H2And 20.20g analytical pure ferric nitrate (Fe (NO O)3)3·9H2O)；
(2) by above-mentioned 4 kinds of raw materials, being dissolved in 150mL distilled water, add 2g Polyethylene Glycol, supersound process makes it disperse
Uniformly, mixed solution russet is obtained；
Step 2: reaction of formation presoma；
Mixed solution russet is placed in four-hole boiling flask, water bath with thermostatic control 40 DEG C, stirs with 180r/min rotating speed continuous uniform；
In four-hole boiling flask, drip the sodium hydroxide solution of 2mol/L, the pH=10 of regulation mixed solution simultaneously；
Step 3, ageing:
By precursors, at room temperature static ageing 8h, remove section top clear liquid, obtain lower floor's thick ageing liquid；
Step 4, crystallization:
(1) by thick for lower floor ageing liquid, concussion shakes up, and moves into teflon-lined hydro-thermal autoclave；
(2) by hydro-thermal autoclave, in the cabinet-type electric furnace of 180 DEG C, crystallization 8h, obtain crystallization liquid；
Step 5, sucking filtration:
Crystallization liquid is cooled to room temperature, respectively washs 4 times with distilled water and dehydrated alcohol, make solution the most neutral, vacuum filtration,
Obtain filter cake；
Step 6, dries and grinds:
(1) filter cake is dried in the drying baker of 80 DEG C, obtain pitchy block；
(2) pitchy block is ground to powder body, i.e. obtains the Ni-Zn ferrite nano materials of cation doping.
Ni prepared by the present embodiment0.6Zn0.15Co0.25Fe2O4The Ni-Zn ferrite nano materials of cation doping, scanning electron microscopic picture is shown in attached
Fig. 3, its mean diameter is 20-30nm, and this nickel zinc cobalt ferrites is 3.4 at the pcrmeability real part of 3GHz Frequency point, and imaginary part is
3.2；Real part of permittivity is 7.5, and imaginary part is 0.17.
Embodiment 3
The preparation method of the Ni-Zn ferrite nano materials of a kind of cation doping, comprises the following steps:
Step 1, dispensing:
(1) Ni is pressed0.4Zn0.4Co0.2Fe2O4Stoichiometric proportion, weighs 4 kinds of raw materials respectively: 2.91g analytical pure nickel nitrate
(Ni(NO3)2·6H2O), 2.97g analytical pure zinc nitrate (Zn (NO3)2·6H2O), 1.46g analytical pure cobalt nitrate
(Co(NO3)2·6H2And 20.20g analytical pure ferric nitrate (Fe (NO O)3)3·9H2O)；
(2) by above-mentioned 4 kinds of raw materials, being dissolved in 150mL distilled water, add 2g Polyethylene Glycol, supersound process makes it disperse
Uniformly, mixed solution russet is obtained；
Step 2: reaction of formation presoma；
Mixed solution russet is placed in four-hole boiling flask, water bath with thermostatic control 45 DEG C, stirs with 150r/min rotating speed continuous uniform
Mix；In four-hole boiling flask, drip the sodium hydroxide solution of 1.5mol/L, the pH=9 of regulation mixed solution simultaneously；
Step 3, ageing:
By precursors, at room temperature static ageing 8h, remove section top clear liquid, obtain lower floor's thick ageing liquid；
Step 4, crystallization:
(1) by thick for lower floor ageing liquid, concussion shakes up, and moves into teflon-lined hydro-thermal autoclave；
(2) by hydro-thermal autoclave, in the cabinet-type electric furnace of 200 DEG C, crystallization 12h, obtain crystallization liquid；
Step 5, sucking filtration:
Crystallization liquid is cooled to room temperature, respectively washs 4 times with distilled water and dehydrated alcohol, make solution the most neutral, vacuum filtration,
Obtain filter cake；
Step 6, dries and grinds:
(1) filter cake is dried in the drying baker of 70 DEG C, obtain pitchy block；
(2) pitchy block is ground to powder body, i.e. obtains the Ni-Zn ferrite nano materials of cation doping.
Ni prepared by the present embodiment0.4Zn0.4Co0.2Fe2O4The Ni-Zn ferrite nano materials of cation doping, scanning electron microscopic picture is shown in accompanying drawing
4, its mean diameter is 20-30nm, and this nickel zinc cobalt ferrites is 3.0 at the pcrmeability real part of 3GHz Frequency point, and imaginary part is 2.8；
Real part of permittivity is 7., and imaginary part is 0.15.
Embodiment 4
The preparation method of the Ni-Zn ferrite nano materials of a kind of cation doping, comprises the following steps:
Step 1, dispensing:
(1) Ni is pressed.05Zn0.35Co0.15Fe2O4Stoichiometric proportion, weighs 4 kinds of raw materials respectively: 3.64g analytical pure nickel nitrate
(Ni(NO3)2·6H2O), 2.60g analytical pure zinc nitrate (Zn (NO3)2·6H2O), 1.09g analytical pure cobalt nitrate
(Co(NO3)2·6H2And 20.20g analytical pure ferric nitrate (Fe (NO O)3)3·9H2O)；
(2) by above-mentioned 4 kinds of raw materials, being dissolved in 150mL distilled water, add 2g Polyethylene Glycol, supersound process makes it disperse
Uniformly, mixed solution russet is obtained；
Step 2: reaction of formation presoma；
Mixed solution russet is placed in four-hole boiling flask, water bath with thermostatic control 35 DEG C, stirs with 240r/min rotating speed continuous uniform
Mix；In four-hole boiling flask, drip the sodium hydroxide solution of 3mol/L, the pH=12 of regulation mixed solution simultaneously；
Step 3, ageing:
By precursors, at room temperature static ageing 6h, remove section top clear liquid, obtain lower floor's thick ageing liquid；
Step 4, crystallization:
(1) by thick for lower floor ageing liquid, concussion shakes up, and moves into teflon-lined hydro-thermal autoclave；
(2) by hydro-thermal autoclave, in the cabinet-type electric furnace of 220 DEG C, crystallization 10h, obtain crystallization liquid；
Step 5, sucking filtration:
Crystallization liquid is cooled to room temperature, respectively washs 4 times with distilled water and dehydrated alcohol, make solution the most neutral, vacuum filtration,
Obtain filter cake；
Step 6, dries and grinds:
(1) filter cake is dried in the drying baker of 80 DEG C, obtain pitchy block；
(2) pitchy block is ground to powder body, i.e. obtains the Ni-Zn ferrite nano materials of cation doping.
Ni prepared by the present embodiment0.5Zn0.35Co0.15Fe2O4The Ni-Zn ferrite nano materials of cation doping, scanning electron microscopic picture is shown in attached
Fig. 5, its mean diameter is 20-30nm, and this nickel zinc cobalt ferrites is 2.9 at the pcrmeability real part of 3GHz Frequency point, and imaginary part is
2.8；Real part of permittivity is 7.1, and imaginary part is 0.16.
Embodiment 5
The preparation method of the Ni-Zn ferrite nano materials of a kind of cation doping, comprises the following steps:
Step 1, dispensing:
(1) Ni is pressed0.5Zn0.3Co0.2Fe2O4Stoichiometric proportion, weighs 4 kinds of raw materials respectively: 3.64g analytical pure nickel nitrate
(Ni(NO3)2·6H2O), 2.23g analytical pure zinc nitrate (Zn (NO3)2·6H2O), 1.46g analytical pure cobalt nitrate
(Co(NO3)2·6H2And 20.20g analytical pure ferric nitrate (Fe (NO O)3)3·9H2O)；
(2) by above-mentioned 4 kinds of raw materials, being dissolved in 150mL distilled water, add 2g Polyethylene Glycol, supersound process makes it disperse
Uniformly, mixed solution russet is obtained；
Step 2: simultaneously carry out (1) and (2), reaction of formation presoma；
Mixed solution russet is placed in four-hole boiling flask, water bath with thermostatic control 50 DEG C, stirs with 180r/min rotating speed continuous uniform
Mix；In four-hole boiling flask, drip the sodium hydroxide solution of 2.5mol/L, the pH=11 of regulation mixed solution simultaneously；
Step 3, ageing:
By precursors, at room temperature static ageing 7h, remove section top clear liquid, obtain lower floor's thick ageing liquid；
Step 4, crystallization:
(1) by thick for lower floor ageing liquid, concussion shakes up, and moves into teflon-lined hydro-thermal autoclave；
(2) by hydro-thermal autoclave, in the cabinet-type electric furnace of 190 DEG C, crystallization 9h, obtain crystallization liquid；
Step 5, sucking filtration:
Crystallization liquid is cooled to room temperature, respectively washs 4 times with distilled water and dehydrated alcohol, make solution the most neutral, vacuum filtration,
Obtain filter cake；
Step 6, dries and grinds:
(1) filter cake is dried in the drying baker of 80 DEG C, obtain pitchy block；
(2) pitchy block is ground to powder body, i.e. obtains the Ni-Zn ferrite nano materials of cation doping.
Ni prepared by the present embodiment0.5Zn0.3Co0.2Fe2O4The Ni-Zn ferrite nano materials of cation doping, scanning electron microscopic picture is shown in accompanying drawing
6, its mean diameter is 20-30nm, and this nickel zinc cobalt ferrites is 3.1 at the pcrmeability real part of 3GHz Frequency point, and imaginary part is 2.9；
Real part of permittivity is 6.9, and imaginary part is 0.15.
Embodiment 6
The preparation method of the Ni-Zn ferrite nano materials of a kind of cation doping, comprises the following steps:
Step 1, dispensing:
(1) Ni is pressed0.6Zn0.35Co0.05Fe2O4Stoichiometric proportion, weighs 4 kinds of raw materials respectively: 4.36g analytical pure nickel nitrate
(Ni(NO3)2·6H2O), 2.60g analytical pure zinc nitrate (Zn (NO3)2·6H2O), 0.36g analytical pure cobalt nitrate
(Co(NO3)2·6H2And 20.20g analytical pure ferric nitrate (Fe (NO O)3)3·9H2O)；
(2) by above-mentioned 4 kinds of raw materials, being dissolved in 150mL distilled water, add 2g Polyethylene Glycol, supersound process makes it disperse
Uniformly, mixed solution russet is obtained；
Step 2: reaction of formation presoma；
Mixed solution russet is placed in four-hole boiling flask, water bath with thermostatic control 40 DEG C, stirs with 270r/min rotating speed continuous uniform
Mix；In four-hole boiling flask, drip the sodium hydroxide solution of 1mol/L, the pH=10 of regulation mixed solution simultaneously；
Step 3, ageing:
By precursors, at room temperature static ageing 9h, remove section top clear liquid, obtain lower floor's thick ageing liquid；
Step 4, crystallization:
(1) by thick for lower floor ageing liquid, concussion shakes up, and moves into teflon-lined hydro-thermal autoclave；
(2) by hydro-thermal autoclave, in the cabinet-type electric furnace of 180 DEG C, crystallization 7h, obtain crystallization liquid；
Step 5, sucking filtration:
Crystallization liquid is cooled to room temperature, respectively washs 4 times with distilled water and dehydrated alcohol, make solution the most neutral, vacuum filtration,
Obtain filter cake；
Step 6, dries and grinds:
(1) filter cake is dried in the drying baker of 70 DEG C, obtain pitchy block；
(2) pitchy block is ground to powder body, i.e. obtains the Ni-Zn ferrite nano materials of cation doping.
Ni prepared by the present embodiment0.6Zn0.35Co0.05Fe2O4The Ni-Zn ferrite nano materials of cation doping, scanning electron microscopic picture is shown in attached
Fig. 7, its mean diameter is 20-30nm, and this nickel zinc cobalt ferrites is 2.9 at the pcrmeability real part of 3GHz Frequency point, and imaginary part is
2.6；Real part of permittivity is 6.9, and imaginary part is 0.14.
Embodiment 7
The preparation method of the Ni-Zn ferrite nano materials of a kind of cation doping, comprises the following steps:
Step 1, dispensing:
(1) Ni is pressed0.5Zn0.25Co0.25Fe2O4Stoichiometric proportion, weighs 4 kinds of raw materials respectively: 3.64g analytical pure nickel nitrate
(Ni(NO3)2·6H2O), 1.86g analytical pure zinc nitrate (Zn (NO3)2·6H2O), 1.82g analytical pure cobalt nitrate
(Co(NO3)2·6H2And 20.20g analytical pure ferric nitrate (Fe (NO O)3)3·9H2O)；
(2) by above-mentioned 4 kinds of raw materials, being dissolved in 150mL distilled water, add 2g Polyethylene Glycol, supersound process makes it disperse
Uniformly, mixed solution russet is obtained；
Step 2: reaction of formation presoma；
Mixed solution russet is placed in four-hole boiling flask, water bath with thermostatic control 45 DEG C, stirs with 210r/min rotating speed continuous uniform
Mix；In four-hole boiling flask, drip the sodium hydroxide solution of 2mol/L, the pH=9 of regulation mixed solution simultaneously；
Step 3, ageing:
By precursors, at room temperature static ageing 7h, remove section top clear liquid, obtain lower floor's thick ageing liquid；
Step 4, crystallization:
(1) by thick for lower floor ageing liquid, concussion shakes up, and moves into teflon-lined hydro-thermal autoclave；
(2) by hydro-thermal autoclave, in the cabinet-type electric furnace of 210 DEG C, crystallization 12h, obtain crystallization liquid；
Step 5, sucking filtration:
Crystallization liquid is cooled to room temperature, respectively washs 4 times with distilled water and dehydrated alcohol, make solution the most neutral, vacuum filtration,
Obtain filter cake；
Step 6, dries and grinds:
(1) filter cake is dried in the drying baker of 60 DEG C, obtain pitchy block；
(2) pitchy block is ground to powder body, i.e. obtains the Ni-Zn ferrite nano materials of cation doping.
Ni prepared by the present embodiment0.5Zn0.25Co0.25Fe2O4The Ni-Zn ferrite nano materials of cation doping, scanning electron microscopic picture is shown in attached
Fig. 8, its mean diameter is 20-30nm, and this nickel zinc cobalt ferrites is 3.3 at the pcrmeability real part of 3GHz Frequency point, and imaginary part is
3.0；Real part of permittivity is 7.3, and imaginary part is 0.17.
Embodiment 8
The preparation method of the Ni-Zn ferrite nano materials of a kind of cation doping, comprises the following steps:
Step 1, dispensing:
(1) Ni is pressed0.6Zn0.2Co0.2Fe2O4Stoichiometric proportion, weighs 4 kinds of raw materials respectively: 4.36g analytical pure nickel nitrate
(Ni(NO3)2·6H2O), 1.49g analytical pure zinc nitrate (Zn (NO3)2·6H2O), 1.46g analytical pure cobalt nitrate
(Co(NO3)2·6H2And 20.20g analytical pure ferric nitrate (Fe (NO O)3)3·9H2O)；
(2) by above-mentioned 4 kinds of raw materials, being dissolved in 150mL distilled water, add 2g Polyethylene Glycol, supersound process makes it disperse
Uniformly, mixed solution russet is obtained；
Step 2: reaction of formation presoma；
Mixed solution russet is placed in four-hole boiling flask, water bath with thermostatic control 40 DEG C, stirs with 150r/min rotating speed continuous uniform
Mix；In four-hole boiling flask, drip the sodium hydroxide solution of 3mol/L, the pH=12 of regulation mixed solution simultaneously；
Step 3, ageing:
By precursors, at room temperature static ageing 6h, remove section top clear liquid, obtain lower floor's thick ageing liquid；
Step 4, crystallization:
(1) by thick for lower floor ageing liquid, concussion shakes up, and moves into teflon-lined hydro-thermal autoclave；
(2) by hydro-thermal autoclave, in the cabinet-type electric furnace of 170 DEG C, crystallization 11h, obtain crystallization liquid；
Step 5, sucking filtration:
Crystallization liquid is cooled to room temperature, respectively washs 4 times with distilled water and dehydrated alcohol, make solution the most neutral, vacuum filtration,
Obtain filter cake；
Step 6, dries and grinds:
(1) filter cake is dried in the drying baker of 80 DEG C, obtain pitchy block；
(2) pitchy block is ground to powder body, i.e. obtains the Ni-Zn ferrite nano materials of cation doping.
Ni prepared by the present embodiment0.6Zn0.2Co0.2Fe2O4The Ni-Zn ferrite nano materials of cation doping, scanning electron microscopic picture is shown in accompanying drawing
9, its mean diameter is 20-30nm, and this nickel zinc cobalt ferrites is 3.2 at the pcrmeability real part of 3GHz Frequency point, and imaginary part is 2.9；
Real part of permittivity is 7.2, and imaginary part is 0.16.
Claims (8)
1. the preparation method of the Ni-Zn ferrite nano materials of a cation doping, it is characterised in that comprise the following steps:
Step 1, dispensing:
(1) Ni is pressedxZnyCo(1-x-y)Fe2O4Stoichiometric proportion, weighs 4 kinds of raw materials respectively: nickel nitrate, zinc nitrate, cobalt nitrate and
Ferric nitrate, wherein, 0.75≤x+y≤0.95,0.4≤x≤0.6,0.15≤y≤0.4；
(2) by above-mentioned 4 kinds of raw materials, it is dissolved in distilled water, adds surfactant, after being uniformly dispersed, obtain russet
Mixed solution；Wherein, in mass ratio, 4 kinds of raw materials quality and: distilled water=(25～28): (150～200), 4 kinds of raw materials quality
With: surfactant=(25～28): (1～3)；
Step 2: reaction of formation presoma；
Mixed solution russet is placed in four-hole boiling flask, water bath with thermostatic control 30～50 DEG C, continues with 150～270r/min rotating speeds
Uniform stirring；In four-hole boiling flask, drip the sodium hydroxide solution of 1～3mol/L, the pH=9～12 of regulation mixed solution simultaneously；
Step 3, ageing:
By precursors, in the static ageing of room temperature 6～10h, remove section top clear liquid, obtain lower floor's thick ageing liquid；
Step 4, crystallization:
(1) by thick for lower floor ageing liquid, concussion shakes up, and moves into teflon-lined hydro-thermal autoclave；
(2) by hydro-thermal autoclave, at 160～220 DEG C, crystallization 6～12h, obtain crystallization liquid；
Step 5, sucking filtration:
Crystallization liquid is cooled to room temperature, and the solution washing obtained, to neutrality, vacuum filtration, obtains filter cake；
Step 6, dries and grinds:
(1) by filter cake 60～80 DEG C of drying, pitchy block is obtained；
(2) pitchy block is ground to powder body, i.e. obtains the Ni-Zn ferrite nano materials of cation doping.
The preparation method of the Ni-Zn ferrite nano materials of cation doping the most according to claim 1, it is characterised in that described step
In rapid 1 (1), nickel nitrate, zinc nitrate, cobalt nitrate and ferric nitrate are analytical pure.
The preparation method of the Ni-Zn ferrite nano materials of cation doping the most according to claim 1, it is characterised in that described step
In rapid 1 (2), surfactant is Polyethylene Glycol.
The preparation method of the Ni-Zn ferrite nano materials of cation doping the most according to claim 1, it is characterised in that described step
In rapid 1 (2), supersound process is used to make it be uniformly dispersed.
The preparation method of the Ni-Zn ferrite nano materials of cation doping the most according to claim 1, it is characterised in that described step
In rapid 2 (2), the speed of dropping sodium hydroxide solution is 0.5～1 drop/sec.
The preparation method of the Ni-Zn ferrite nano materials of cation doping the most according to claim 1, it is characterised in that described step
In 4 (2), crystallization is carried out in cabinet-type electric furnace.
The preparation method of the Ni-Zn ferrite nano materials of cation doping the most according to claim 1, it is characterised in that described step
In rapid 5, use distilled water and absolute ethanol washing.
The preparation method of the Ni-Zn ferrite nano materials of cation doping the most according to claim 1, it is characterised in that described step
In rapid 6 (1), air dry oven is used to dry.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109037961A (en) * | 2018-07-11 | 2018-12-18 | 长江大学 | A kind of nickel-zinc ferrite absorbing material and preparation method thereof |
| CN110683796A (en) * | 2019-11-25 | 2020-01-14 | 惠州市中为柔性光电子智能制造研究院有限公司 | Inhomogeneous metamaterial for converging electromagnetic waves |
| CN114053966A (en) * | 2021-03-04 | 2022-02-18 | 中国科学院宁波材料技术与工程研究所 | Hydrophilic magnetic nano material and preparation method and application thereof |
| CN116134001A (en) * | 2020-03-31 | 2023-05-16 | 西布列塔尼大学 | Method for producing nickel zinc cobalt spinel ferrite in ceramic form |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105016395A (en) * | 2015-06-29 | 2015-11-04 | 深圳顺络电子股份有限公司 | Nano ferrite material, and preparation method thereof |
| CN105060872A (en) * | 2015-07-24 | 2015-11-18 | 天长市中德电子有限公司 | High-impedance low-power-consumption soft magnetic ferrite material and preparation method thereof |
-
2016
- 2016-05-11 CN CN201610311768.XA patent/CN106006751B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105016395A (en) * | 2015-06-29 | 2015-11-04 | 深圳顺络电子股份有限公司 | Nano ferrite material, and preparation method thereof |
| CN105060872A (en) * | 2015-07-24 | 2015-11-18 | 天长市中德电子有限公司 | High-impedance low-power-consumption soft magnetic ferrite material and preparation method thereof |
Non-Patent Citations (6)
| Title |
|---|
| F. GOZÜAK, ET AL.: "Synthesis and characterization of CoxZn1-xFe2O4 magnetic nanoparticles via a PEG-assisted route", 《JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS》 * |
| HÜSEYIN KAVAS, ET AL.: "Cation distribution and magnetic properties of Zn doped NiFe2O4 nanoparticles synthesized by PEG-assisted hydrothermal route", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| M. SERTKOL, ET AL.: "Synthesis and magnetic characterization of Zn0.6Ni0.4Fe2O4 nanoparticles via a polyethylene glycol-assisted hydrothermal route", 《JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS》 * |
| NERMIN KASAPOGLU, ET AL.: "Synthesis and magnetic properties of octahedral ferrite NixCo1-xFe2O4 nanocrystals", 《CENTRAL EUROPEAN JOURNAL OF CHEMISTRY》 * |
| 刘晓霞等: "镍锌钴铁氧体/碳纳米管复合吸波材料的制备及表征", 《化工新型材料》 * |
| 唐培朵等: "镍锌钴铁氧体的水热低温合成与高频电磁性能研究", 《材料导报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109037961A (en) * | 2018-07-11 | 2018-12-18 | 长江大学 | A kind of nickel-zinc ferrite absorbing material and preparation method thereof |
| CN110683796A (en) * | 2019-11-25 | 2020-01-14 | 惠州市中为柔性光电子智能制造研究院有限公司 | Inhomogeneous metamaterial for converging electromagnetic waves |
| CN116134001A (en) * | 2020-03-31 | 2023-05-16 | 西布列塔尼大学 | Method for producing nickel zinc cobalt spinel ferrite in ceramic form |
| CN114053966A (en) * | 2021-03-04 | 2022-02-18 | 中国科学院宁波材料技术与工程研究所 | Hydrophilic magnetic nano material and preparation method and application thereof |
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