CN105161246A - Nickel-zinc ferrite/polyacrylic acid nano-composite material and preparation method thereof - Google Patents

Nickel-zinc ferrite/polyacrylic acid nano-composite material and preparation method thereof Download PDF

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CN105161246A
CN105161246A CN201510519492.XA CN201510519492A CN105161246A CN 105161246 A CN105161246 A CN 105161246A CN 201510519492 A CN201510519492 A CN 201510519492A CN 105161246 A CN105161246 A CN 105161246A
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nickel
composite material
zinc ferrite
ferrite
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CN105161246B (en
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罗驹华
高多多
姚为
王旭
姜翠凤
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Yangcheng Institute of Technology
Yancheng Institute of Technology
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Abstract

The invention discloses a nickel-zinc ferrite/polyacrylic acid nano-composite material and a preparation method thereof. The nano-composite material is in a core-shell structure and comprises core nickel-zinc ferrite and shell polyacrylic acid; the shell polyacrylic acid coats the nickel-zinc ferrite; and the nano-composite material is represented by Ni0.1-1Zn0.1-1Fe1-3O2-6/PAA. The preparation method of the nano-composite material mainly comprises the following steps: (1) weighing zinc sulfate, ferrous sulfate and nickel sulfate to prepare a metal salt solution, adding the metal salt solution into an ammonium oxalate solution; (2) adjusting the pH of the mixed solution, and separating and drying the mixed solution to obtain a ferrite precursor; (3) burning the ferrite precursor to obtain the nickel-zinc ferrite; and (4) mixing and reacting the nickel-zinc ferrite and acrylic acid, and separating and drying the mixture to obtain the nickel-zinc ferrite/polyacrylic acid nano-composite material. The nickel-zinc ferrite/polyacrylic acid nano-composite material has the advantages of low specific saturated magnetic field intensity, relatively low coercive force and relatively high soft magnetic property; and the preparation method disclosed by the invention is simple, feasible and low in cost.

Description

A kind of nickel-zinc ferrite/sodium polyacrylate nano composite material and preparation method thereof
Technical field
The invention belongs to field of nanocomposite materials, particularly relate to a kind of nickel-zinc ferrite/sodium polyacrylate nano composite material and preparation method thereof.
Background technology
A kind of multiphase solid material that nano composite material is made up of two or more physics or the different material of chemical property, wherein has one at least at one-dimensional square to being be in nano level particulate, crystal grain, film or fiber; And newly-generated solid phase material has the physics different from common large scale material or chemical property.Nano composite material generally can be divided into by solid-phase component: inorganic nano composite material, Organic/Inorganic Composite Nanomaterials, organic/organic nanocomposite.Due to the nanophase comprised in nano composite material, so there is a large amount of interfaces between matrix and reinforcement, reinforcement.Its structural particularity, nano composite material is made to possess the effect of some uniquenesses, mainly small-size effect and surperficial or interfacial effect, thus in performance, the difference of highly significant is had with the micro materials on the traditional concept of same composition, show the performance of many excellences and brand-new function, show wide application prospect in a lot of fields.
Magnetic nanometer composite material is a class new function composite material of development in recent years, according to the composition of magnetic nanometer composite material, magnetic nanometer composite material can be divided into inorganic magnetic nano composite material (to comprise metal system magnetic nanometer composite material, ferrite magnetic nano composite material, magnetic Nano composite granules film etc.), high polymer magnetic nanometer composite material (comprises natural high polymer magnetic nanometer composite material, Prof. Du Yucang high polymer magnetic nanometer composite material etc.) and magnetic fluid (iron oxygen magnetic fluid, metal MHD, nitrogenize magnetic fluid etc.) three classes.
Soft magnetic ferrite is that current purposes is wide, wide in variety, and quantity is large, a kind of Ferrite Material that the output value is high.It is mainly used as various inductance element, as filter magnetic core, magnetic core of transformer, radio magnetic core and tape recording and video recording head etc., also be the critical material of magnetic recording element, ferronickel ferrite is the electronics industry and mechanotronics basic material that a kind of purposes is wide, output is large, cost is low.At present, along with electronic product develops to miniaturization, preparation density soft magnetic ferrite that is high, uniform small grains is particularly important, but this material is under more weak magnetic field, easy magnetization also easily demagnetizes, as zinc chrome ferrite and nickel-zinc ferrite etc., because the magnetic energy stored in ferrite unit volume is lower, full close the magnetization also lower (usually only having the 1/3-1/5 of pure iron), thus limit its application in the low frequency forceful electric power required compared with high magnetic energy density and high-power field.Therefore, the research of soft magnetic ferrite nano composite material becomes one of focus of research both at home and abroad.
Summary of the invention
Goal of the invention: the present invention first object is to provide a kind of nickel zinc-iron/sodium polyacrylate nano composite material with high soft magnetic characteristic; The second object of the present invention is to provide the preparation method of this nano composite material.
Technical scheme: nickel-zinc ferrite of the present invention/sodium polyacrylate nano composite material is nucleocapsid structure, be preferably spherical particle, this nucleocapsid structure comprises the shell polyacrylic acid of kernel nickel-zinc ferrite and coated nickel-zinc ferrite, this material Ni 0.1 ~ 1zn 0.1 ~ 1fe 1 ~ 3o 2 ~ 6/ PAA represents, can be preferably Ni 0.5zn 0.5fe 2o 4/ PAA.
The present invention adopts following steps to prepare this nickel-zinc ferrite/sodium polyacrylate nano composite material:
(1) according to Ni 0.1 ~ 1zn 0.1 ~ 1fe 1 ~ 3o 2 ~ 6stoichiometric proportion 0.1 ~ 1:0.1 ~ 1:1 ~ 3 weigh nickelous sulfate, zinc sulfate, ferrous sulfate preparing metal salting liquid respectively, configuration concentration is the ammonium oxalate solution of 0.5 ~ 1.5mol/L, after this ammonium oxalate solution is heated to 30 ~ 50 DEG C, and add metal salt solution wherein, wherein, the volume ratio of ammonium oxalate solution and metal salt solution is 2:1, then insulated and stirred mixed solution.Preferably, Ni 0.1 ~ 1zn 0.1 ~ 1fe 1 ~ 3o 2 ~ 6stoichiometric proportion 0.5 ~ 1:0.5 ~ 1:2 ~ 3.
(2) pH of mixed solution is regulated to be 9 ~ 12 by the NaOH solution of 6 ~ 8mol/L.
(3) by mixed solution centrifugation, obtain after sediment, adopt deionized water and washes of absolute alcohol sediment 2 ~ 3 times respectively.Furtherly, the rotating speed 5000r/min of centrifugation, time interval 10min.
(4) by dry under vacuum for the sediment after cleaning, ferrite presoma is obtained.Furtherly, this drying is dry 12 ~ 24h under 40 ~ 80 DEG C of vacuum conditions.
(5) this ferrite presoma is calcined 9 ~ 11h under 100 ~ 300 DEG C of conditions, then calcine 1 ~ 3h under being warmed up to 700 ~ 900 DEG C of conditions, obtain nickel-zinc ferrite.Preferably, this ferrite presoma is calcined 10 ~ 11h under 200 ~ 300 DEG C of conditions, then calcine 2 ~ 3h under being warmed up to 800 ~ 900 DEG C of conditions.First step precalcining can make ferrite nucleation, the calcining of second step, makes ferrite nucleating growth, obtains the magnetic ferrite of tool, and the ferrite compactness that this calcining manners obtains is good, best in quality.
(6) nickel-zinc ferrite obtained is disperseed in deionized water, add acrylic acid and heat 1 ~ 3h under 50 ~ 80 DEG C of water bath condition, add initator simultaneously, dispersant and crosslinking agent, wherein, nickel-zinc ferrite, acrylic acid, initator, the mass ratio of dispersant and crosslinking agent is 0.1 ~ 1:10 ~ 40:0.01 ~ 0.05:0.1 ~ 0.5:3 ~ 8, after reaction terminates, centrifugation product obtains sediment, adopt deionized water and washes of absolute alcohol sediment 2 ~ 3 times respectively, under 40 ~ 80 DEG C of vacuum conditions, dry 12 ~ 24h obtains nickel-zinc ferrite/sodium polyacrylate nano composite material.Preferably, the mass ratio of this nickel-zinc ferrite, acrylic acid, initator, dispersant and crosslinking agent is 0.4 ~ 0.6:25 ~ 35:0.02 ~ 0.04:0.2 ~ 0.4:4 ~ 6; Meanwhile, initator can be ammonium persulfate, and dispersant can be isopropyl alcohol, and crosslinking agent can be glutaraldehyde.
Beneficial effect: compared with prior art, remarkable advantage of the present invention is that nickel zinc-iron/sodium polyacrylate nano composite material has obvious nucleocapsid structure, hysteresis is there is under externally-applied magnetic field, be far smaller than ferritic than saturation magnetic field intensity than saturation magnetic field intensity, coercive force is less, there is higher soft magnetic characteristic, it is desirable soft magnetic material, can be used as various inductance element, as filter magnetic core, magnetic core of transformer, radio magnetic core, and tape recording and video recording head etc., be also the critical material of magnetic recording element.Meanwhile, preparation method's materials of the present invention are simple, and preparation technology is easy and simple to handle, and without the need to the synthesis device of complexity, preparation cost is lower.
Accompanying drawing explanation
Fig. 1 is the XRD figure of NiZn ferrite presoma (a) and NiZn ferrite (b) through 800 DEG C of calcining 2h;
Fig. 2 is Ni 0.5zn 0.5fe 2o 4(a) and Ni 0.5zn 0.5fe 2o 4the infrared spectrogram of/PAA (b);
Fig. 3 is the Ni that 800 DEG C of calcining 2h obtain 0.5zn 0.5fe 2o 4the magnetic hysteresis loop of powder;
Fig. 4 is Ni 0.5zn 0.5fe 2o 4the magnetic hysteresis loop of/PAA composite material;
Fig. 5 is Ni 0.5zn 0.5fe 2o 4tEM figure;
Fig. 6 is Ni 0.5zn 0.5fe 2o 4the TEM figure of/PAA.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is described further.
Nickel zinc-iron/sodium polyacrylate nano composite material of the present invention is nucleocapsid structure, comprises the shell polyacrylic acid of kernel nickel-zinc ferrite and coated nickel-zinc ferrite, this composite material Ni 0.1 ~ 1zn 0.1 ~ 1fe 1 ~ 3o 2 ~ 6/ PAA represents, preferably, this composite material can be Ni 0.5zn 0.5fe 2o 4/ PAA.
The preparation method of nickel zinc-iron/sodium polyacrylate nano composite material of the present invention, comprises the steps:
(1) according to Ni 0.1 ~ 1zn 0.1 ~ 1fe 1 ~ 3o 2 ~ 6stoichiometric proportion 0.1 ~ 1:0.1 ~ 1:1 ~ 3 weigh nickelous sulfate, zinc sulfate, ferrous sulfate preparing metal salting liquid respectively, configuration concentration is the ammonium oxalate solution of 0.5 ~ 1.5mol/L, after this ammonium oxalate solution is heated to 30 ~ 50 DEG C, add metal salt solution wherein, wherein, the volume ratio of ammonium oxalate solution and metal salt solution is 2:1, then insulated and stirred mixed solution, preferably, Ni 0.1 ~ 1zn 0.1 ~ 1fe 1 ~ 3o 2 ~ 6stoichiometric proportion 0.5 ~ 1:0.5 ~ 1:2 ~ 3.
(2) pH of mixed solution is regulated to be 9 ~ 12 by the NaOH solution of 6 ~ 8mol/L;
(3) after mixed solution centrifugation being obtained sediment, adopt deionized water and washes of absolute alcohol sediment 2 ~ 3 times respectively, furtherly, the rotating speed of centrifugation is 5000r/min, the time interval is 10min, and this rotating speed and the time interval are conducive to mixed solution and are separated fully;
(4) by the dry 12 ~ 24h under 40 ~ 80 DEG C of vacuum conditions of the sediment after cleaning, ferrite presoma is obtained.
(5) ferrite presoma is calcined 9 ~ 11h under 100 ~ 300 DEG C of conditions, then calcine 1 ~ 3h under being warmed up to 700 ~ 900 DEG C of conditions, obtain nickel-zinc ferrite.
(6) nickel-zinc ferrite obtained is disperseed in deionized water, add acrylic acid and heat 1 ~ 3h under 50 ~ 80 DEG C of water bath condition, add simultaneously and send out agent ammonium persulfate, isopropyl alcohol dispersant, crosslinking agent glutaraldehyde, wherein, nickel-zinc ferrite, acrylic acid, initator, the mass ratio of dispersant and crosslinking agent is 0.1 ~ 1:10 ~ 40:0.01 ~ 0.05:0.1 ~ 0.5:3 ~ 8, after reaction terminates, centrifugation product obtains sediment, adopt deionized water and washes of absolute alcohol sediment 2 ~ 3 times respectively, under 40 ~ 80 DEG C of vacuum conditions, dry 12 ~ 24h obtains nickel-zinc ferrite/sodium polyacrylate nano composite material, preferably, nickel-zinc ferrite, acrylic acid, initator, the mass ratio of dispersant and crosslinking agent is 0.4 ~ 0.6:25 ~ 35:0.02 ~ 0.04:0.2 ~ 0.4:4 ~ 6.
Embodiment 1
(1) according to Ni 0.5zn 0.5fe 2o 4stoichiometric proportion 0.5:0.5:2 weigh nickelous sulfate, zinc sulfate, ferrous sulfate preparing metal salting liquid respectively, configuration concentration is the ammonium oxalate solution of 1.0mol/L, after this ammonium oxalate solution is heated to 40 DEG C, metal salt solution is added to it, wherein, the volume ratio of ammonium oxalate solution and metal salt solution is 2:1, then insulated and stirred mixed solution.
(2) pH of mixed solution is regulated to be 10 by the NaOH solution of 7mol/L;
(3) by mixed solution centrifugation, the rotating speed of centrifugation is 5000r/min, and the time interval is 10min, obtains after sediment, adopts deionized water and washes of absolute alcohol sediment 2 times respectively.
(4) by the sediment dry 24h under 60 DEG C of vacuum conditions after cleaning, ferrite presoma is obtained.
(5) ferrite presoma is calcined 10 hours under 200 DEG C of conditions, then calcine 2 hours under 800 DEG C of conditions, naturally namely obtain required nickel-zinc ferrite after cooling;
(6) beaker that nickel-zinc ferrite 0.5g puts into 100ml is taken, add the distilled water of 60ml, ultrasonic wave process 2h makes it fully disperse, then the acrylic monomers measuring 30ml adds the above-mentioned aqueous solution, under 65 DEG C of water bath condition, heat 2h, simultaneously according to the mass ratio 0.5:30:0.03:0.3:5 of the addition of ferrite, acrylic acid, initator, dispersant and crosslinking agent, add initiator ammonium persulfate, isopropyl alcohol dispersant and crosslinking agent glutaraldehyde, constantly stir; After question response terminates, product centrifugation obtained after sediment, with deionized water and absolute ethanol washing sediment 3 times, finally dry 24h under 60 DEG C of vacuum conditions, obtains Ni 0.5zn 0.5fe 2o 4/ PAA nano composite material.
The experimental result of embodiment 1 represents:
Fig. 1 is NiZn ferrite presoma (a) and the NiZn ferritic XRD figure through 800 DEG C of calcining 2h, and from Fig. 1 (a), diffraction peaks broadening is comparatively serious, this is because crystallite dimension is less and crystallization degree is lower.In figure (b), 2 θ values are 27.28 °, 39.08 °, 44.54 °, 53.08 °, 64.96 °, 66.91 °, the diffraction maximum of the characteristic diffraction peak of 73.46 ° and 84.78 ° (111), (220), (311) of corresponding nickel-zinc ferrite, (400), (422), (511), (440) and (620) crystal face respectively, the width of diffraction maximum and the relative intensity at peak are all consistent with standard diagram JCPDS standard, powder is crystalline state, in spinel cubic crystalline structure.
Fig. 2 is Ni 0.5zn 0.5fe 2o 4(a) and Ni 0.5zn 0.5fe 2o 4the infrared spectrogram of/PAA (b).
In figure (a), owing to there is adsorbed water molecule, so sample is at 3440cm -1and 1632cm -1near there is the characteristic peak of H-O-H, 577cm -1and 420cm -1there is Ni in place 0.5zn 0.5fe 2o 4characteristic peak.
In figure (b), can find out at 1710cm -1neighbouring strong absworption peak demonstrates the existence of-COOH; Composite material is at 1582cm -1appearance new peak, place, 1411cm -1the relative intensity at peak, place increases.At 1600cm -1the neighbouring peak occurred is the asymmetric stretching vibration of R-COO-, at 1400cm -1the neighbouring peak occurred is the symmetrical stretching vibration of R-COO-, and this shows to there occurs chemical reaction between a part of carboxyl of PAA and ferrite.
Fig. 3 is the Ni nanoparticle that 800 DEG C of calcining 2h obtain 0.5zn 0.5fe 2o 4the magnetic hysteresis loop of powder, as can be seen from Figure 3, prepared ferrite powder creates closed magnetic hysteresis loop.Can find out, when applied field strengths little with 1500Oe time, the magnetization of sample enlarges markedly along with the increase of applied field strengths, slowly increases, until reach capacity when electric field strength is greater than 1500Oe along with the increase of applied field strengths.Ni 0.5zn 0.5fe 2o 4powder saturation magnetization is 68.14emug -1, coercive force, for being approximately zero, presents superparamagnetism.
Fig. 4 is Ni nanoparticle 0.5zn 0.5fe 2o 4the magnetic hysteresis loop of/PAA composite material.As seen from Figure 4, composite material exhibits goes out obvious ferromagnetism, and the saturation magnetization of composite nanoparticle is 6.83emug -1, coercive force is for being approximately zero.The saturation magnetization of composite material obviously reduces.
Fig. 5 is Ni 0.5zn 0.5fe 2o 4tEM figure.As can be seen from Figure 5, most of Ni 0.5zn 0.5fe 2o 4the particle diameter of nano particle is at about 40nm, and particle dispersion is better, and ferrite particle is substantially spherical in shape, and its particle diameter is relatively more even, but has also occurred reunion to a certain degree.
Fig. 6 is Ni 0.5zn 0.5fe 2o 4the TEM figure of/PAA nano composite material.As can be seen from Figure 6, composite particles microscopic pattern mostly is spherical particle, and particle kernel and outside border exist obvious contrast difference, shows that central spherical particle and outside border present and wraps up and wrapped relation, form obvious morphology of core-shell structure.What color was lighter is the polyacrylic acid forming shell, and saturate is the ferrite nano particles forming core.
Embodiment 2
Step is substantially the same manner as Example 1, and difference is: the mass ratio of nickel-zinc ferrite, acrylic acid, initator, dispersant and crosslinking agent is 0.1:40:0.01:0.5:8.
Embodiment 3
Step is substantially the same manner as Example 1, and difference is: the mass ratio of nickel-zinc ferrite, acrylic acid, initator, dispersant and crosslinking agent is 1:10:0.05:0.1:3.
The performance comparison table of nickel-zinc ferrite prepared by table 1 embodiment 1-3/sodium polyacrylate nano composite material
As shown in Table 1, nickel-zinc ferrite/sodium polyacrylate the nano composite material of embodiment 1 gained is better than embodiment 2 and embodiment 3 in saturation magnetization, soft magnetism and coercive force performance, this be with the chemical bonding effect between the dispersity of nickel-zinc ferrite nano particle in polyacrylic acid, organic and inorganic to the surface nature of ferrite particle and the change of microstructure and polymer relevant to factors such as the coating functions of inorganic nano-particle.When polyacrylic acid is excessive, integument is blocked up, produce shielding action, otherwise do not reach coated effect, organic and inorganic Interaction Force weakens, and all can affect saturation magnetization and coercive force, thus changes ferritic magnetic property.
Embodiment 4
Step is substantially the same manner as Example 1, and difference is: in step (1), according to Ni 0.1zn 0.1fe 3o 6stoichiometric proportion 0.1:0.1:3 weigh zinc sulfate, ferrous sulfate, nickelous sulfate preparing metal salting liquid respectively, configuration concentration is the ammonium oxalate solution of 0.5mol/L; In step (2), the concentration of NaOH solution is 8mol/L, regulates pH to be 9; In step (4), by the sediment dry 24h under 40 DEG C of vacuum conditions after cleaning; Ferrite presoma is calcined 11h in (5) by step under 100 DEG C of conditions, then calcines 3h under being warmed up to 700 DEG C of conditions; In step (6), the mass ratio of nickel-zinc ferrite, acrylic acid, initator, dispersant and crosslinking agent is 0.4:35:0.02:0.4:4, under 50 DEG C of water bath condition, heat 3h, drying 12 under 80 DEG C of vacuum conditions.
Embodiment 5
Step is substantially the same manner as Example 1, and difference is: in step (1), according to NiZnFeO 2stoichiometric proportion 1:1:1 weigh nickelous sulfate, zinc sulfate, ferrous sulfate preparing metal salting liquid respectively, configuration concentration is the ammonium oxalate solution of 1.5mol/L; In step (2), the concentration of NaOH solution is 6mol/L, regulates pH to be 12; In step (4), by the sediment dry 12h under 80 DEG C of vacuum conditions after cleaning; Ferrite presoma is calcined 9h in (5) by step under 300 DEG C of conditions, then calcines 1h under being warmed up to 900 DEG C of conditions; In step (6), the mass ratio of nickel-zinc ferrite, acrylic acid, initator, dispersant and crosslinking agent is 0.6:25:0.04:0.2:6, under 80 DEG C of water bath condition, heat 1h, dry 24h under 40 DEG C of vacuum conditions.
Embodiment 6
Design 9 groups of parallel tests, Ni 0.1 ~ 1zn 0.1 ~ 1fe 1 ~ 3o 2 ~ 6middle Ni, Zn, Fe stoichiometric proportion is respectively (0.5:0.5:2), (0.1:0.1:3), (1:1:1), (0.05:0.5:2), (1.2:0.5:2), (0.5:0.05:2), (0.5:1.2:2), (0.5:0.5:0.5), (0.5:0.5:3.2).Preparation method is identical with embodiment 1.
The performance comparison table of the nickel-zinc ferrite/sodium polyacrylate nano composite material of table 2 different chemical metering ratio
As shown in Table 2, saturation magnetization and the coercive force performance of embodiment 1-3 are better than embodiment 4-9, wherein work as Ni 0.1 ~ 1zn 0.1 ~ 1fe 1 ~ 3o 2 ~ 6stoichiometric proportion when 0.1 ~ 1:0.1 ~ 1:1 ~ 3, the performance of the composite material of gained is relatively better; Again stoichiometrically than being the best during 0.5:0.5:2.Because coercive force is relevant with grain size, in embodiment 1, products therefrom diffraction maximum is the strongest, and crystallization is the most complete, and crystal formation is the most perfect, and crystallite dimension is large, and coercive force, closer to 0, has higher soft magnet performance; The diffraction peak intensity of other components is more weak relative to the former with crystallite dimension may be because its surface has the enhancing that more dangling bonds cause surface magnetic anisotropy, makes ionic bonding effect symmetry on the surface poor, makes product have higher coercive force.

Claims (10)

1. nickel-zinc ferrite/sodium polyacrylate nano composite material, is characterized in that: this nano composite material is nucleocapsid structure, comprises the shell polyacrylic acid of kernel nickel-zinc ferrite and coated nickel-zinc ferrite, uses Ni 0.1 ~ 1zn 0.1 ~ 1fe 1 ~ 3o 2 ~ 6/ PAA represents.
2. nickel-zinc ferrite according to claim 1/sodium polyacrylate nano composite material, is characterized in that: described nano composite material Ni 0.5zn 0.5fe 2o 4/ PAA represents.
3. prepare a method for nickel-zinc ferrite according to claim 1/sodium polyacrylate nano composite material, it is characterized in that comprising the steps:
(1) with nickelous sulfate, zinc sulfate, ferrous sulfate for raw material stoichiometrically 0.1 ~ 1:0.1 ~ 1:1 ~ 3 preparing metal salting liquid, configuration concentration is the ammonium oxalate solution of 0.5 ~ 1.5mol/L, after this ammonium oxalate solution is heated to 30 ~ 50 DEG C, and add metal salt solution wherein, wherein, the volume ratio of described ammonium oxalate solution and metal salt solution is 2:1, then insulated and stirred mixed solution;
(2) pH of described mixed solution is regulated to be 9 ~ 12 by NaOH solution;
(3) by described mixed solution centrifugation, after obtaining sediment, with washing agent washing and precipitating thing;
(4) by dry under vacuum for the sediment after cleaning, ferrite presoma is obtained;
(5) this ferrite presoma is calcined 9 ~ 11h under 100 ~ 300 DEG C of conditions, then calcine 1 ~ 3h under being warmed up to 700 ~ 900 DEG C of conditions, obtain nickel-zinc ferrite;
(6) nickel-zinc ferrite obtained is disperseed in deionized water, add acrylic acid to carry out adding thermal response, add initator, dispersant and crosslinking agent simultaneously, wherein, the mass ratio of described nickel-zinc ferrite, acrylic acid, initator, dispersant and crosslinking agent is 0.1 ~ 1:10 ~ 40:0.01 ~ 0.05:0.1 ~ 0.5:3 ~ 8, after reaction terminates, centrifugation product obtains sediment, with washing agent washing and precipitating thing, drying obtains nickel-zinc ferrite/sodium polyacrylate nano composite material.
4. prepare the method for nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterized in that: in step (1), described zinc sulfate, nickelous sulfate, ferrous sulfate are raw material stoichiometrically 0.5 ~ 1:0.5 ~ 1:2 ~ 3 preparing metal salting liquid.
5. prepare the method for nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterized in that: in step (5), described ferrite presoma is calcined 10 ~ 11h under 200 ~ 300 DEG C of conditions, calcine 2 ~ 3h under being warmed up to 800 ~ 900 DEG C of conditions, obtain described nickel-zinc ferrite.
6. prepare the method for nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterized in that: in step (6), the mass ratio of described nickel-zinc ferrite, acrylic acid, initator, dispersant and crosslinking agent is 0.4 ~ 0.6:25 ~ 35:0.02 ~ 0.04:0.2 ~ 0.4:4 ~ 6.
7. prepare the method for nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterized in that: in step (3) and step (6), described is adopt deionized water and absolute ethanol washing 2 ~ 3 times respectively with washing agent washing and precipitating thing.
8. prepare the method for nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterized in that: in step (4) and step (6), described drying is dry 12 ~ 24h under 40 ~ 80 DEG C of vacuum conditions.
9. prepare the method for nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterized in that: in step (6), described in be heated to be heating water bath, wherein, heating-up temperature is 50 ~ 80 DEG C, and heating time is 1 ~ 3h.
10. prepare the method for nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterized in that: in step (6), described initator is ammonium persulfate, and dispersant is isopropyl alcohol, and crosslinking agent is glutaraldehyde.
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CN113135596A (en) * 2021-04-15 2021-07-20 中国恩菲工程技术有限公司 Method for preparing soft magnetic ferrite precursor by coprecipitation method
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CN113461071A (en) * 2021-06-10 2021-10-01 贵州理工学院 Method for preparing nickel-zinc ferrite from waste nickel-hydrogen waste battery
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