CN103396110A - Barium titanate-nickel zinc ferrite composite ceramic material and preparation method thereof - Google Patents
Barium titanate-nickel zinc ferrite composite ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a barium titanate-nickel zinc ferrite composite ceramic material and a preparation method thereof. The barium titanate-nickel zinc ferrite composite ceramic material comprises a barium titanate phase and a nickel zinc ferrite phase, the barium titanate phase is coated by the nickel zinc ferrite phase, and the molar percentage content of the nickel zinc ferrite phase is 33 mol %-91 mol %. In the barium titanate-nickel zinc ferrite composite ceramic material, advantages of nickel zinc ferrite and barium titanate are composited, the barium titanate phase is coated by the nickel zinc ferrite phase, and the molar percentage content of the nickel zinc ferrite phase is 33 mol %-91 mol %, so that the nickel zinc ferrite and the barium titanate are not simply superposed; the magnetic property can be improved due to the continuity of the nickel zinc ferrite as a magnetic medium, so that a high magnetic permeability can be ensured, dielectric properties also can be improved, and the magnetic permeability and dielectric properties of the barium titanate-nickel zinc ferrite composite ceramic material are high.
Description
Technical field
The present invention relates to electric capacity, inductance Amphoteric Materials technical field, particularly relate to a kind of barium titanate-nickel zinc ferrite composite ceramic material and preparation method thereof.
Background technology
Single-phase how ferromagnetic electroceramics material is subjected to the restriction of its structure, and seldom, and its performance is not good has greatly limited its application for number.Ferromagnetic-ferroelectric composite ceramic material can make up the inferior position of single-phase how ferromagnetic electroceramics material aspect of performance greatly.Along with electronic encapsulation device miniaturization, high-performance, multi-functional being integrated in one and requirement cheaply, the research of ferromagnetic-Ferroelectric Composites becomes the focus that everybody falls over each other to study further, can be applied in the multifunction devices such as some wave filters, sensor and signal processor unit.
At present, the method for the ferromagnetic-ferroelectric ceramic material of preparation generally adopts solid sintering technology.Yet there is its intrinsic inferior position in solid sintering technology, for example, and high energy consumption, higher to equipment requirements; As raw material, the metal oxide cost is higher, be unfavorable for cost control with metal oxide; The purity of the product for preparing is larger to the final performance impact of product; In mechanical milling process, metal oxide particle easily produces the autohemagglutination phenomenon; Ion diffusion in high temperature sintering, produce lattice distortion, makes all decreases to some degree of magnetic, dielectric properties.
Summary of the invention
, based on this, be necessary to provide a kind of magnetic permeability and the higher barium titanate-nickel zinc ferrite composite ceramic material of dielectric properties.
A kind of preparation method of barium titanate-nickel zinc ferrite composite ceramic material further, is provided.
A kind of barium titanate-nickel zinc ferrite composite ceramic material, comprise barium titanate phase and nickel-zinc ferrite phase, and described nickel-zinc ferrite coats described barium titanate phase mutually, and the molar content of described nickel-zinc ferrite phase is 33mol%～91mol%.
In embodiment, the molar content of described nickel-zinc ferrite phase is 60mol%～67mol% therein.
A kind of preparation method of barium titanate-nickel zinc ferrite composite ceramic material, comprise the steps:
1:1:4 obtains zinc salt, nickel salt and iron salt dissolved the mixing solutions of zinc salt, nickel salt and molysite in deionized water in molar ratio, and described mixing solutions is heated to 60 ℃～80 ℃;
It is in the mixing solutions of 60 ℃～80 ℃ that barium titanate is added described temperature, obtains the mixture of mixing solutions and barium titanate after mixing, and wherein, the mol ratio of described barium titanate and described molysite is 1:1～1:20;
The pH value of described mixture is adjusted to 8～11, gets precipitation after reacting completely, the described barium titanate-nickel zinc ferrite presoma that is precipitated as;
After described barium titanate-nickel zinc ferrite presoma drying, pre-burning, calcining is 2 hours～4 hours under 600 ℃～1000 ℃, obtains the barium titanate-nickel zinc ferrite composite granule;
Add tackiness agent in described barium titanate-nickel zinc ferrite composite granule, after compression moulding, in 900 ℃～1200 ℃ lower sintering 2 hours～4 hours, obtain the barium titanate-nickel zinc ferrite composite ceramic material after cooling, described barium titanate-nickel zinc ferrite composite ceramic material comprises barium titanate phase and nickel-zinc ferrite phase, described nickel-zinc ferrite coats described barium titanate phase mutually, and the molar content of described nickel-zinc ferrite phase is 33mol%～91mol%.
In embodiment, after described barium titanate-nickel zinc ferrite presoma drying, before pre-burning, comprise the step of grinding and sieving therein; Add tackiness agent in described barium titanate-nickel zinc ferrite composite granule, also comprise the step of grinding and sieving before the step of compression moulding.
In embodiment, after described compression moulding, also comprised the step of pre-burning before 900 ℃～1200 ℃ lower sintering step of 2 hours～4 hours therein, the temperature of described pre-burning is 300 ℃～500 ℃, and the pre-burning time is 2 hours.
In embodiment, described zinc salt is zinc acetate, zinc nitrate or zinc chloride therein, and described nickel salt is nickel acetate, nickelous nitrate or nickelous chloride, and described molysite is ferric sulfate, iron nitrate or iron(ic) chloride.
In embodiment, the particle diameter of described barium titanate is 50 nanometers～400 nanometers therein.
Therein in embodiment, it is described that barium titanate is added described temperature is in the mixing solutions of 60 ℃～80 ℃, before obtaining the mixture of mixing solutions and barium titanate after mixing, also comprise described barium titanate is washed, then in 700 ℃～1000 ℃ calcinings step of 2 hours.
Therein in embodiment, the pH value of described mixture being adjusted to 8～11 step is to add strong base solution that the pH value of described mixture is adjusted to 8～11 to described mixture.
In embodiment, described strong base solution is the aqueous solution of sodium hydroxide or the aqueous solution of potassium hydroxide therein.
In embodiment, the described time that reacts completely is 4 hours～6 hours therein.
In embodiment, described tackiness agent is the aqueous solution of polyvinyl alcohol therein, and the mass ratio of polyvinyl alcohol and water is 6:100～8:100.
in above-mentioned barium titanate-nickel zinc ferrite composite ceramic material, it is high that nickel-zinc ferrite has a high frequency magnetic permeability, low-loss, the advantage of high resistivity and good stability in use, barium titanate has high dielectric, low-loss and eco-friendly advantage, the barium titanate-nickel zinc ferrite composite ceramic material combines the advantage of nickel-zinc ferrite and barium titanate, and, nickel-zinc ferrite coats the barium titanate phase mutually, the molar content of nickel-zinc ferrite phase is 33mol%～91mol%, making barium titanate and nickel-zinc ferrite is not simple superposition, the continuity of this magnetic medium of nickel-zinc ferrite has improved magnetic property, therefore can guarantee high magnetic permeability, also can realize the raising of dielectric properties, make magnetic permeability and the dielectric properties of barium titanate-nickel zinc ferrite composite ceramic material higher.
Description of drawings
Fig. 1 is preparation method's the schema of the barium titanate-nickel zinc ferrite composite ceramic material of an embodiment;
Fig. 2 is the XRD figure of the nickel-zinc ferrite stupalith of embodiment 1 preparation;
Fig. 3 is the XRD figure of the barium titanate ceramics material of embodiment 2 preparations;
Fig. 4 is the scanning electron microscope (SEM) photograph of the barium titanate-nickel zinc ferrite composite ceramic material of embodiment 3 preparations;
Fig. 5 is the XRD figure of the barium titanate-nickel zinc ferrite composite ceramic material of embodiment 3 preparations;
Fig. 6 is the frequency-permeability curcve of the barium titanate-nickel zinc ferrite composite ceramic material of the barium titanate ceramics material of embodiment 2 and embodiment 3～7;
Fig. 7 is the frequency-specific inductivity curve of the barium titanate-nickel zinc ferrite composite ceramic material of the barium titanate ceramics material of nickel-zinc ferrite stupalith, embodiment 2 of embodiment 1 and embodiment 3～7.
Embodiment
, for above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.A lot of details have been set forth in the following description so that fully understand the present invention.But the present invention can implement much to be different from alternate manner described here, and those skilled in the art can be in the situation that do similar improvement without prejudice to intension of the present invention, so the present invention is not subjected to the restriction of following public concrete enforcement.
The barium titanate-nickel zinc ferrite composite ceramic material of one embodiment, comprise barium titanate phase and nickel-zinc ferrite phase, and wherein, nickel-zinc ferrite coats the barium titanate phase mutually, and the molar content of nickel-zinc ferrite phase is 33mol%～91mol%.
Nickel-zinc ferrite has advantages of the high and low loss of high frequency magnetic permeability, high resistivity and good stability in use.In the barium titanate-nickel zinc ferrite composite ceramic material, nickel-zinc ferrite is as magnetic medium.Nickel-zinc ferrite coats the barium titanate phase mutually, keeps the continuity of magnetic medium, and the continuity of magnetic medium has promoter action to the raising of this composite ceramic material magnetic property, can guarantee higher magnetic permeability.And due to the semiconduction matter of nickel-zinc ferrite, the barium titanate-nickel zinc ferrite composite ceramic material has certain seep effect aspect dielectric.
Barium titanate has high dielectric, low-loss and eco-friendly advantage, and barium titanate has higher frequency stability.Molar content is that the barium titanate of 9mol%～67% can improve frequency stability and the dielectric properties to the barium titanate-nickel zinc ferrite composite ceramic material.
The barium titanate-nickel zinc ferrite composite ceramic material combines the advantage of nickel-zinc ferrite and barium titanate, and, nickel-zinc ferrite coats the barium titanate phase mutually, the molar content of nickel-zinc ferrite phase is 33mol%～91mol%, nickel-zinc ferrite and barium titanate are not simple superposition, the continuity of this magnetic medium of nickel-zinc ferrite has improved magnetic property, therefore can guarantee high magnetic permeability, also can realize the raising of dielectric properties, make the magnetic permeability of barium titanate-nickel zinc ferrite composite ceramic material and dielectric properties higher.The performance of the barium titanate-nickel zinc ferrite composite ceramic material of this structure be better than that barium titanate and nickel-zinc ferrite simple superposition form the barium titanate-nickel zinc ferrite composite ceramic material.
Preferably, the molar content of nickel-zinc ferrite phase is 60mol%～67mol%.The results showed, when the molar content of nickel-zinc ferrite phase was 60mol%～67mol%, no matter from dielectric properties, magnetic permeability and quality factor aspect, the performance of barium titanate-nickel zinc ferrite composite ceramic material was more excellent.
The results showed, in 10MHz～1GHz range of frequency, this barium titanate-nickel zinc ferrite composite ceramic material limiting frequency f
rImprove, magnetic loss reduces, initial permeability μ
iSignificantly improve with the quality factor q product, have high-k and high magnetic permeability, can be used for wave filter, signal processor unit.
See also Fig. 1, the preparation method of an embodiment barium titanate-nickel zinc ferrite composite ceramic material, comprise the steps:
Step S110: 1:1:4, with obtaining the mixing solutions of zinc salt, nickel salt and molysite in zinc salt, nickel salt and iron salt dissolved deionized water, is heated to 60 ℃～80 ℃ with mixing solutions in molar ratio.
Zinc salt is preferably zinc acetate (Zn (CH
3COO)
22H
2O), zinc nitrate (Zn (NO
3)
26H
2O) or zinc chloride (ZnCl
26H
2O).
Nickel salt is preferably nickel acetate (Ni (CH
3COO)
29H
2O), nickelous nitrate (Ni (NO
3)
26H
2O) or nickelous chloride (NiCl
26H
2O).
Molysite is preferably ferric sulfate (Fe
2(SO
4)
39H
2O), iron nitrate (Fe (NO
3)
39H
2O) or iron(ic) chloride (FeCl
36H
2O).
In above-mentioned these several zinc salts, nickel salt and molysite water soluble, and with respect to the metal oxide that high temperature solid-state method adopts, price is lower, is conducive to reduce the price of the barium titanate-nickel zinc ferrite composite ceramic material for preparing.
The mode of heating is preferably heating in water bath.The mixing solutions of zinc salt, nickel salt and molysite is heated to 60 ℃～80 ℃, so that subsequent reactions.
The consumption of deionized water should guarantee fully to dissolve zinc salt, nickel salt and molysite, and the barium titanate-nickel zinc ferrite presoma of follow-up generation is had enough carrying capacities.Generally for the barium titanate-nickel zinc ferrite presoma that generates 0.025mol, the amount of deionized water is 80ml～100ml.
Step S120: it is in the mixing solutions of 60 ℃～80 ℃ that barium titanate is added temperature, obtains the mixture of mixing solutions and barium titanate after mixing, and wherein, the mol ratio of barium titanate and molysite is 1:1～1:20.
The particle diameter of barium titanate is 50 nanometers～400 nanometers.Using particle diameter is the nano barium carbonate of 50 nanometers～400 nanometers, is conducive to barium titanate on the one hand dispersed, is conducive on the other hand follow-up nickel-zinc ferrite and coats mutually the barium titanate phase.
Preferably, it is in the mixing solutions of 60 ℃～80 ℃ that barium titanate is added temperature, obtain after mixing mixture before, the step that barium titanate is washed and calcines.After barium titanate water successively and washing with alcohol, in 700 ℃～1000 ℃ calcinings 2 hours.Barium titanate successively water and washing with alcohol to wash away impurity and surface and oil contaminant.In 700 ℃～1000 ℃ calcinings 2 hours, to obtain the barium titanate of Tetragonal, the barium titanate dielectric properties of Tetragonal were higher.
It is in the mixing solutions of 60 ℃～80 ℃ that barium titanate after the calcining amount that is 1:1～1:20 by the mol ratio with molysite is added temperature, obtains mixing solutions and barium titanate mixture after mixing.
Step S130: the pH value of mixture is adjusted to 8～11, gets precipitation after reacting completely, be precipitated as the barium titanate-nickel zinc ferrite presoma.
Drip strong base solution to mixture, the 20w%～30w% of the amount excess theory value of the strong base solution that drips, take the pH value of regulating mixture as 8～11.Theoretical value is the amount of the required highly basic of oxyhydroxide that generates fully according to molysite, nickel salt, zinc salt.
The pH value of regulating mixture is 8～11, so that zinc salt, nickel salt and molysite generate respectively the oxyhydroxide of zinc, the oxyhydroxide of nickel and the oxyhydroxide of iron, and guarantees that zinc salt, nickel salt and molysite generate precipitation of hydroxide fully.Simultaneously, be under 8～11 environment, to guarantee that the oxyhydroxide of nickel, zinc and iron can stable existence at pH.
Preferably, strong base solution is that concentration is the aqueous solution of sodium hydroxide of 8mol/L or the aqueous solution of potassium hydroxide.
Drip in the strong base solution process, constantly stir, after dripping, stirring reaction 4 hours～6 hours, make and react completely, make zinc salt, nickel salt and molysite generate respectively the oxyhydroxide of zinc, the oxyhydroxide of nickel and the oxyhydroxide of iron, then reactant is cooled to room temperature, vacuum filtration, be precipitated, repeatedly to neutrality, with washing with alcohol once, obtain the barium titanate-nickel zinc ferrite presoma with the deionized water washing precipitation.
Step S140: after barium titanate-nickel zinc ferrite presoma drying, pre-burning, calcining is 2 hours～4 hours under 600 ℃～1000 ℃, obtains the barium titanate-nickel zinc ferrite composite granule.
The barium titanate-nickel zinc ferrite presoma that step S130 is obtained is in the baking oven of 60 ℃ after dry 24 hours and pre-burning, and then calcining 2 hours～4 hours under 600 ℃～1000 ℃, obtain the barium titanate-nickel zinc ferrite composite granule.
Preferably, the temperature of pre-burning is 300 ℃～500 ℃, and the pre-burning time is 2 hours.
For the follow-up less barium titanate-nickel zinc ferrite matrix material of particle diameter that obtains, before the pre-burning of dried barium titanate-nickel zinc ferrite presoma, also comprise the step of grinding and sieving, after grinding, with 400 mesh sieve, sieve.
Step S150: add tackiness agent in the barium titanate-nickel zinc ferrite composite granule, after compression moulding,, in 900 ℃～1200 ℃ lower sintering 2 hours～4 hours, obtain the barium titanate-nickel zinc ferrite composite ceramic material after cooling.
Tackiness agent is preferably the aqueous solution of polyvinyl alcohol.The aqueous solution of polyvinyl alcohol is added in the barium titanate-nickel zinc ferrite composite granule, after evenly mixing, grind granulation, compression moulding.
Preferably, in the aqueous solution of polyvinyl alcohol, the mass ratio of polyvinyl alcohol and water is 6:100～8～100.The quality of polyvinyl alcohol account for the barium titanate-nickel zinc ferrite composite granule quality 8%～12%.
In other embodiments, also can adopt polyvinyl butyral acetal solution as tackiness agent.But, because polyvinyl alcohol is water-soluble, adopt the aqueous solution of polyvinyl alcohol as tackiness agent, environmental protection, and inexpensive.
With the barium titanate-nickel zinc ferrite composite granule after compression moulding in 900 ℃～1200 ℃ lower sintering 2 hours～4 hours, the reaction of barium titanate-nickel zinc ferrite composite granule generates the barium titanate-nickel zinc ferrite composite ceramic material, this barium titanate-nickel zinc ferrite composite ceramic material comprises barium titanate phase and nickel-zinc ferrite phase, wherein, nickel-zinc ferrite coats the barium titanate phase mutually, and the molar content of nickel-zinc ferrite phase is 33mol%～91mol%.
Preferably, add tackiness agent in the barium titanate-nickel zinc ferrite composite granule, also comprise the step of grinding and sieving before the step of compression moulding, after grinding, with 400 mesh sieve, sieve.
Preferably, after the compression moulding of barium titanate-nickel zinc ferrite composite granule, also comprised the step of pre-burning before 900 ℃～1200 ℃ lower sintering step of 2 hours～4 hours, the temperature of pre-burning is 300 ℃～500 ℃, and the pre-burning time is 2 hours.
Prior to 300 ℃～500 ℃ lower pre-burnings after 2 hours again in 900 ℃～1200 ℃ lower sintering 2 hours～4 hours, be conducive to form the higher crystallization of quality.
The preparation method's of above-mentioned barium titanate-nickel zinc ferrite composite ceramic material reaction conditions is gentleer, and preparation time is shorter, and adjunct is few, and preparation-obtained barium titanate-nickel zinc ferrite composite ceramic material purity is higher, and crystallinity is better.
Adopt nickel salt, zinc salt, molysite to substitute nickel oxide, zinc oxide, ferric oxide, greatly reduce its production cost; And adopt the mode of water dissolution and co-precipitation, can get rid of in traditional high temperature solid-state method, due to the different metal oxides uneven problem of dispersion that the intergranular mutual repulsion effect of different metal is brought in mechanical milling process for the first time.Barium titanate adds in mixing solutions, when reducing energy consumption, can improve the dispersiveness of barium titanate.
Adopt deionized water as solvent, environment-protecting asepsis, operating procedure aspect are more easily implemented.
Below further set forth by specific embodiment.
Prepare the nickel-zinc ferrite stupalith
(1) taking 10.905g Nickelous nitrate hexahydrate, 11.1559g zinc nitrate hexahydrate and 60.6g Fe(NO3)39H2O is dissolved in the there-necked flask of 300ml deionized water, be placed in 80 ℃ of heating in water bath, mechanical stirring, to dissolving, obtains the mixing solutions of zinc salt, nickel salt and molysite;
(2) aqueous solution 100ml of the sodium hydroxide of preparation 8mol/L, dropwise join the aqueous solution of sodium hydroxide in above-mentioned mixing solutions with separating funnel, and the limit edged stirs, until it dropwises, the pH value of regulating mixing solutions is 9.Then continue stirring reaction 4h, complete to precipitation, the question response thing is cooled to room temperature, is poured into Büchner funnel and carries out vacuum filtration, and the employing deionized water wash repeatedly to neutrality, with washing with alcohol once, obtains the nickel-zinc ferrite presoma;
(3) with nickel-zinc ferrite presoma dry 24h in the baking oven of 60 ℃, then grind, re-use 400 mesh sieve and sieve and obtain powder, this powder is put into crucible and is placed in retort furnace, in 500 ℃ of pre-burning 2h, then, in 600 ℃ of calcining 4h, cool to room temperature with the furnace and obtain nickel-zinc ferrite powder;
(4) nickel-zinc ferrite powder sieves with 400 mesh sieve, the aqueous solution (mass ratio of polyethylene alcohol and water is 8:100) that adds polyvinyl alcohol, wherein, the quality of the aqueous solution of polyvinyl alcohol is the quality 8% of nickel-zinc ferrite powder, grinds granulation, compression moulding, in 300 ℃ of pre-burning 2h,, in 900 ℃ of sintering 4h, cool to room temperature with the furnace again, obtain the nickel-zinc ferrite stupalith.
Fig. 2 is the XRD figure of above-mentioned nickel-zinc ferrite stupalith.Can draw from Fig. 2, the nickel-zinc ferrite stupalith has significantly and Ni
0.5Zn
0.5Fe
2O
4The consistent spinel structure of standard card (PDF:52-0178), its characteristic peak 2 θ=30.0126 °, 35.538 °, 62.585 ° and Miller indices (022), (113), (044) is perfect corresponding.In addition, sharp and strong peak crystallization explanation ferrite powder has crystallization phases preferably.
Prepare barium titanate ceramics material
(1) be to carry out drying after the barium titanate powder of 400 nanometers washs successively with deionized water and ethanol with particle diameter, then in 700 ℃ of calcining 2h;
(2) get barium titanate powder after above-mentioned calcining, add the aqueous solution (mass ratio of polyethylene alcohol and water is 8:100) of the polyvinyl alcohol of its quality 8%, grind granulation, compression moulding, in 400 ℃ of pre-burning 2h, then with 900 ℃ of sintering 4h, cool to room temperature with the furnace, obtain barium titanate ceramics material.
Fig. 3 is the XRD figure of barium titanate ceramics material.Can draw from Fig. 3, barium titanate ceramics material has the significantly perovskite structure consistent with barium titanate standard card (PDF:76-0744), its characteristic peak 2 θ=31.651 °, 38.893 °, 45.371 °, 56.275 ° of standards are corresponding to Miller index (110), (111), (200), (211) its peak shows that by force its degree of crystallinity is better, and purity is higher.
Embodiment 3
Prepare the barium titanate-nickel zinc ferrite composite ceramic material
(1) take 8.2302g zinc acetate, 9.3323g nickelous acetate and 42.141 ferric sulfate and dissolve in the there-necked flask of 300ml deionized water, be placed in 80 ℃ of heating in water bath, mechanical stirring, to dissolving, obtains the mixing solutions of zinc salt, nickel salt and molysite;
(2) be to carry out drying after the barium titanate powder of 400 nanometers washs successively with deionized water and ethanol with the 34.9788g particle diameter, then in 700 ℃ of calcining 2h;
(3) barium titanate powder after calcining adds in above-mentioned mixing solutions, obtain the mixture of mixing solutions and barium titanate after mixing, the aqueous solution 100ml of the sodium hydroxide of preparation 8mol/L, dropwise join the aqueous solution of sodium hydroxide in said mixture with separating funnel, the limit edged stirs, until it dropwises, the pH value of regulating mixing solutions is 10.Then continue stirring reaction 4h, complete to precipitation, the question response thing is cooled to room temperature, is poured into Büchner funnel and carries out vacuum filtration, and the employing deionized water wash repeatedly to neutrality, with washing with alcohol once, obtains the barium titanate-nickel zinc ferrite presoma;
(4) with barium titanate-nickel zinc ferrite presoma dry 24h in the baking oven of 60 ℃, then grind, re-using 400 mesh sieve sieves and obtains powder, this powder is put into crucible and is placed in retort furnace, in 500 ℃ of pre-burning 2h,, in 600 ℃ of calcining 4h, cool to room temperature with the furnace and obtain the barium titanate-nickel zinc ferrite powder again;
(5) the barium titanate-nickel zinc ferrite powder sieves with 400 mesh sieve, the aqueous solution (mass ratio of polyethylene alcohol and water is 8:100) that adds polyvinyl alcohol, wherein, the quality of polyvinyl alcohol solution is the quality 8% of nickel-zinc ferrite powder, grind granulation, compression moulding, in 300 ℃ of pre-burning 2h, again in 900 ℃ of sintering 4h, cool to room temperature with the furnace, obtain the barium titanate-nickel zinc ferrite composite ceramic material, this barium titanate-nickel zinc ferrite composite ceramic material comprises barium titanate phase and nickel-zinc ferrite phase, nickel-zinc ferrite coats the barium titanate phase mutually, the molecular fraction of nickel-zinc ferrite phase is 33%.
Fig. 4 is the scanning electron microscope (SEM) photograph of above-mentioned barium titanate-nickel zinc ferrite composite ceramic material.As seen from Figure 4, the surface of this barium titanate-nickel zinc ferrite composite ceramic material forms uniform crystalline particle, and crystallinity is better.
Fig. 5 is the XRD figure of above-mentioned barium titanate-nickel zinc ferrite composite ceramic material.As can be seen from Figure 5, the XRD figure of this barium titanate-nickel zinc ferrite composite ceramic material is the stack of peak shape of the barium titanate ceramics material of the nickel-zinc ferrite stupalith of embodiment 1 and embodiment 2, comprise nickel-zinc ferrite and barium titanate two-phase, purity is better, and degree of crystallinity is high.
Prepare the barium titanate-nickel zinc ferrite composite ceramic material
(1) taking 10.905g Nickelous nitrate hexahydrate, 11.1559g zinc nitrate hexahydrate and 60.6g Fe(NO3)39H2O is dissolved in the there-necked flask of 300ml deionized water, be placed in 60 ℃ of heating in water bath, mechanical stirring, to dissolving, obtains the mixing solutions of zinc salt, nickel salt and molysite;
(2) be to carry out drying after the barium titanate powder of 50 nanometers washs successively with deionized water and ethanol with the 11.6596g particle diameter, then in 900 ℃ of calcining 2h;
(3) barium titanate powder after calcining adds in above-mentioned mixing solutions, obtain the mixture of mixing solutions and barium titanate after mixing, the aqueous solution 100ml of the sodium hydroxide of preparation 8mol/L, dropwise join the aqueous solution of sodium hydroxide in said mixture with separating funnel, the limit edged stirs, until it dropwises, the pH value of regulating mixing solutions is 8.Then continue stirring reaction 6h, complete to precipitation, the question response thing is cooled to room temperature, is poured into Büchner funnel and carries out vacuum filtration, and the employing deionized water wash repeatedly to neutrality, with washing with alcohol once, obtains the barium titanate-nickel zinc ferrite presoma;
(4) with barium titanate-nickel zinc ferrite presoma dry 24h in the baking oven of 60 ℃, then grind, re-using 400 mesh sieve sieves and obtains powder, this powder is put into crucible and is placed in retort furnace, in 300 ℃ of pre-burning 2h,, in 1000 ℃ of calcining 2h, cool to room temperature with the furnace and obtain the barium titanate-nickel zinc ferrite powder again;
(5) the barium titanate-nickel zinc ferrite powder sieves with 400 mesh sieve, the aqueous solution (mass ratio of polyethylene alcohol and water is 7:100) that adds polyvinyl alcohol, wherein, the quality of polyvinyl alcohol solution is the quality 12% of nickel-zinc ferrite powder, grind granulation, compression moulding, in 300 ℃ of pre-burning 2h, again in 1050 ℃ of sintering 4h, cool to room temperature with the furnace, obtain the barium titanate-nickel zinc ferrite composite ceramic material, this barium titanate-nickel zinc ferrite composite ceramic material comprises barium titanate phase and nickel-zinc ferrite phase, nickel-zinc ferrite coats the barium titanate phase mutually, the molecular fraction of nickel-zinc ferrite phase is 60%.
Embodiment 5
Prepare the barium titanate-nickel zinc ferrite composite ceramic material
(1) take 9.1613g zinc chloride, 8.91g nickelous chloride and 40.6025g iron(ic) chloride and be dissolved in the there-necked flask of 300ml deionized water, be placed in 70 ℃ of heating in water bath, mechanical stirring, to dissolving, obtains the mixing solutions of zinc salt, nickel salt and molysite;
(2) be to carry out drying after the barium titanate powder of 300 nanometers washs successively with deionized water and ethanol with the 8.7447g particle diameter, then in 1000 ℃ of calcining 2h;
(3) barium titanate powder after calcining adds in above-mentioned mixing solutions, obtain the mixture of mixing solutions and barium titanate after mixing, the aqueous solution 100ml of the sodium hydroxide of preparation 8mol/L, dropwise join the aqueous solution of sodium hydroxide in said mixture with separating funnel, the limit edged stirs, until it dropwises, the pH value of regulating mixing solutions is 9.Then continue stirring reaction 5h, complete to precipitation, the question response thing is cooled to room temperature, is poured into Büchner funnel and carries out vacuum filtration, and the employing deionized water wash repeatedly to neutrality, with washing with alcohol once, obtains the barium titanate-nickel zinc ferrite presoma;
(4) with barium titanate-nickel zinc ferrite presoma dry 24h in the baking oven of 60 ℃, then grind, re-using 400 mesh sieve sieves and obtains powder, this powder is put into crucible and is placed in retort furnace, in 500 ℃ of pre-burning 2h,, in 800 ℃ of calcining 3h, cool to room temperature with the furnace and obtain the barium titanate-nickel zinc ferrite powder again;
(5) the barium titanate-nickel zinc ferrite powder sieves with 400 mesh sieve, the aqueous solution (mass ratio of polyethylene alcohol and water is 6:100) that adds polyvinyl alcohol, wherein, the quality of polyvinyl alcohol solution is the quality 10% of nickel-zinc ferrite powder, grind granulation, compression moulding, in 400 ℃ of pre-burning 2h, again in 1200 ℃ of sintering 4h, cool to room temperature with the furnace, obtain the barium titanate-nickel zinc ferrite composite ceramic material, this barium titanate-nickel zinc ferrite composite ceramic material comprises barium titanate phase and nickel-zinc ferrite phase, nickel-zinc ferrite coats the barium titanate phase mutually, the molecular fraction of nickel-zinc ferrite phase is 67%.
Prepare the barium titanate-nickel zinc ferrite composite ceramic material
(1) taking 10.905g Nickelous nitrate hexahydrate, 11.1559g zinc nitrate hexahydrate and 60.6g Fe(NO3)39H2O is dissolved in the there-necked flask of 300ml deionized water, be placed in 75 ℃ of heating in water bath, mechanical stirring, to dissolving, obtains the mixing solutions of zinc salt, nickel salt and molysite;
(2) be to carry out drying after the barium titanate powder of 100 nanometers washs successively with deionized water and ethanol with the 3.4979g particle diameter, then in 900 ℃ of calcining 2h;
(3) barium titanate powder after calcining adds in above-mentioned mixing solutions, obtain the mixture of mixing solutions and barium titanate after mixing, the aqueous solution 100ml of the sodium hydroxide of preparation 8mol/L, dropwise join the aqueous solution of sodium hydroxide in said mixture with separating funnel, the limit edged stirs, until it dropwises, the pH value of regulating mixing solutions is 11.Then continue stirring reaction 4h, complete to precipitation, the question response thing is cooled to room temperature, is poured into Büchner funnel and carries out vacuum filtration, and the employing deionized water wash repeatedly to neutrality, with washing with alcohol once, obtains the barium titanate-nickel zinc ferrite presoma;
(4) with barium titanate-nickel zinc ferrite presoma dry 24h in the baking oven of 60 ℃, then grind, re-using 400 mesh sieve sieves and obtains powder, this powder is put into crucible and is placed in retort furnace, in 500 ℃ of pre-burning 2h,, in 1000 ℃ of calcining 4h, cool to room temperature with the furnace and obtain the barium titanate-nickel zinc ferrite powder again;
(5) the barium titanate-nickel zinc ferrite powder sieves with 400 mesh sieve, the aqueous solution (mass ratio of polyethylene alcohol and water is 9:100) that adds polyvinyl alcohol, wherein, the quality of polyvinyl alcohol solution is the quality 9% of nickel-zinc ferrite powder, grind granulation, compression moulding, in 350 ℃ of pre-burning 2h, again in 900 ℃ of sintering 4h, cool to room temperature with the furnace, obtain the barium titanate-nickel zinc ferrite composite ceramic material, this barium titanate-nickel zinc ferrite composite ceramic material comprises barium titanate phase and nickel-zinc ferrite phase, nickel-zinc ferrite coats the barium titanate phase mutually, the molecular fraction of nickel-zinc ferrite phase is 83%.
Embodiment 7
Prepare the barium titanate-nickel zinc ferrite composite ceramic material
(1) taking 10.905g Nickelous nitrate hexahydrate, 11.1559g zinc nitrate hexahydrate and 60.6g Fe(NO3)39H2O is dissolved in the there-necked flask of 300ml deionized water, be placed in 80 ℃ of heating in water bath, mechanical stirring, to dissolving, obtains the mixing solutions of zinc salt, nickel salt and molysite;
(2) be to carry out drying after the barium titanate powder of 200 nanometers washs successively with deionized water and ethanol with the 1.7489g particle diameter, then in 750 ℃ of calcining 2h;
(3) barium titanate powder after calcining adds in above-mentioned mixing solutions, obtain the mixture of mixing solutions and barium titanate after mixing, the aqueous solution 100ml of the sodium hydroxide of preparation 8mol/L, dropwise join the aqueous solution of sodium hydroxide in said mixture with separating funnel, the limit edged stirs, until it dropwises, the pH value of regulating mixing solutions is 9.Then continue stirring reaction 4h, complete to precipitation, the question response thing is cooled to room temperature, is poured into Büchner funnel and carries out vacuum filtration, and the employing deionized water wash repeatedly to neutrality, with washing with alcohol once, obtains the barium titanate-nickel zinc ferrite presoma;
(4) with barium titanate-nickel zinc ferrite presoma dry 24h in the baking oven of 60 ℃, then grind, re-using 400 mesh sieve sieves and obtains powder, this powder is put into crucible and is placed in retort furnace, in 500 ℃ of pre-burning 2h,, in 900 ℃ of calcining 2.5h, cool to room temperature with the furnace and obtain the barium titanate-nickel zinc ferrite powder again;
(5) the barium titanate-nickel zinc ferrite powder sieves with 400 mesh sieve, the aqueous solution (mass ratio of polyethylene alcohol and water is 8:100) that adds polyvinyl alcohol, wherein, the quality of polyvinyl alcohol solution is the quality 8% of nickel-zinc ferrite powder, grind granulation, compression moulding, in 300 ℃ of pre-burning 2h, again in 1100 ℃ of sintering 4h, cool to room temperature with the furnace, obtain the barium titanate-nickel zinc ferrite composite ceramic material, this barium titanate-nickel zinc ferrite composite ceramic material comprises barium titanate phase and nickel-zinc ferrite phase, nickel-zinc ferrite coats the barium titanate phase mutually, the molecular fraction of nickel-zinc ferrite phase is 91%.
Fig. 6 is the frequency-permeability curcve of the barium titanate-nickel zinc ferrite composite ceramic material of the barium titanate ceramics material of embodiment 2 and embodiment 3～7, wherein, curve II～curve VII is respectively the frequency-permeability curcve of the stupalith of embodiment 2 and embodiment 3～7.As seen from Figure 6, in 10MHz～1GHz range of frequency, the magnetic permeability of the barium titanate-nickel zinc ferrite composite ceramic material of embodiment 3～7 is all higher than the magnetic permeability of the barium titanate ceramics material of embodiment 2.And, the magnetic permeability of the barium titanate-nickel zinc ferrite composite ceramic material of embodiment 3～7 increases with the molar fraction of nickel-zinc ferrite phase, and the magnetic permeability of every group of barium titanate-nickel zinc ferrite composite ceramic material roughly presents the trend of first constant rear reduction with frequency.
Fig. 7 is the frequency-specific inductivity curve of the barium titanate-nickel zinc ferrite composite ceramic material of the barium titanate ceramics material of nickel-zinc ferrite stupalith, embodiment 2 of embodiment 1 and embodiment 3～7, wherein, curve I～curve VII is respectively the frequency of the material of embodiment 1～7-specific inductivity curve.As seen from Figure 7, the specific inductivity of the barium titanate-nickel zinc ferrite composite ceramic material of embodiment 3～7 is all greater than the specific inductivity of the nickel-zinc ferrite stupalith of embodiment 1, the specific inductivity of this different materials roughly presents and first reduces the trend that raises afterwards and then reduce with the increase of the molar fraction of nickel-zinc ferrite, be that percolation threshold appears in 60% place in molar fraction, because of adding of barium titanate, specific inductivity changes little with increase frequency.
Table 1 is the limiting frequency f of the barium titanate-nickel zinc ferrite composite ceramic material of the barium titanate ceramics material of nickel-zinc ferrite stupalith, embodiment 2 of embodiment 1 and embodiment 3～7
rThe limiting frequency of barium titanate-nickel zinc ferrite composite ceramic material adds and increases gradually with barium titanate, be 33% in the nickel-zinc ferrite molar fraction, when the barium titanate molar fraction is 67%, its limiting frequency is 11 times of limiting frequency of pure nickel Zn ferrite stupalith, has greatly improved the scope of application of this barium titanate-nickel zinc ferrite composite ceramic material.
Table 2 is that quality factor q and the over-all properties of the barium titanate-nickel zinc ferrite composite ceramic material of the barium titanate ceramics material of nickel-zinc ferrite stupalith, embodiment 2 of embodiment 1 and embodiment 3～7 characterizes μ
i* Q product table.The quality factor q of barium titanate-nickel zinc ferrite composite ceramic material reduces with the increase of nickel-zinc ferrite molar fraction, and characterizes the μ of matrix material Integrated using performance
i* Q product is maximum when the nickel-zinc ferrite molar fraction is 60%.
Table 1
Table 2
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.Should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (12)
1. a barium titanate-nickel zinc ferrite composite ceramic material, is characterized in that, comprises barium titanate phase and nickel-zinc ferrite phase, and described nickel-zinc ferrite coats described barium titanate phase mutually, and the molar content of described nickel-zinc ferrite phase is 33mol%～91mol%.
2. barium titanate-nickel zinc ferrite composite ceramic material according to claim 1, is characterized in that, the molar content of described nickel-zinc ferrite phase is 60mol%～67mol%.
3. the preparation method of a barium titanate-nickel zinc ferrite composite ceramic material, comprise the steps:
1:1:4 obtains zinc salt, nickel salt and iron salt dissolved the mixing solutions of zinc salt, nickel salt and molysite in deionized water in molar ratio, and described mixing solutions is heated to 60 ℃～80 ℃;
It is in the mixing solutions of 60 ℃～80 ℃ that barium titanate is added described temperature, obtains the mixture of mixing solutions and barium titanate after mixing, and wherein, the mol ratio of described barium titanate and described molysite is 1:1～1:20;
The pH value of described mixture is adjusted to 8～11, gets precipitation after reacting completely, the described barium titanate-nickel zinc ferrite presoma that is precipitated as;
After described barium titanate-nickel zinc ferrite presoma drying, pre-burning, calcining is 2 hours～4 hours under 600 ℃～1000 ℃, obtains the barium titanate-nickel zinc ferrite composite granule;
Add tackiness agent in described barium titanate-nickel zinc ferrite composite granule, after compression moulding, in 900 ℃～1200 ℃ lower sintering 2 hours～4 hours, obtain the barium titanate-nickel zinc ferrite composite ceramic material after cooling, described barium titanate-nickel zinc ferrite composite ceramic material comprises barium titanate phase and nickel-zinc ferrite phase, described nickel-zinc ferrite coats described barium titanate phase mutually, and the molar content of described nickel-zinc ferrite phase is 33mol%～91mol%.
4. the preparation method of barium titanate-nickel zinc ferrite composite ceramic material according to claim 3, is characterized in that, after described barium titanate-nickel zinc ferrite presoma drying, before pre-burning, comprises the step of grinding and sieving; Add tackiness agent in described barium titanate-nickel zinc ferrite composite granule, also comprise the step of grinding and sieving before the step of compression moulding.
5. the preparation method of barium titanate-nickel zinc ferrite composite ceramic material according to claim 3, it is characterized in that, after described compression moulding, the step that also comprised pre-burning before 900 ℃～1200 ℃ lower sintering step of 2 hours～4 hours, the temperature of described pre-burning is 300 ℃～500 ℃, and the pre-burning time is 2 hours.
6. the preparation method of barium titanate-nickel zinc ferrite composite ceramic material according to claim 3, it is characterized in that, described zinc salt is zinc acetate, zinc nitrate or zinc chloride, and described nickel salt is nickel acetate, nickelous nitrate or nickelous chloride, and described molysite is ferric sulfate, iron nitrate or iron(ic) chloride.
7. the preparation method of barium titanate-nickel zinc ferrite composite ceramic material according to claim 3, is characterized in that, the particle diameter of described barium titanate is 50 nanometers～400 nanometers.
8. the preparation method of barium titanate-nickel zinc ferrite composite ceramic material according to claim 3, it is characterized in that, it is described that barium titanate is added described temperature is in the mixing solutions of 60 ℃～80 ℃, before obtaining the mixture of mixing solutions and barium titanate after mixing, also comprise described barium titanate is washed, then in 700 ℃～1000 ℃ calcinings step of 2 hours.
9. the preparation method of barium titanate-nickel zinc ferrite composite ceramic material according to claim 3, it is characterized in that, the pH value of described mixture being adjusted to 8～11 step is to add strong base solution that the pH value of described mixture is adjusted to 8～11 to described mixture.
10. the preparation method of barium titanate-nickel zinc ferrite composite ceramic material according to claim 9, is characterized in that, described strong base solution is the aqueous solution of sodium hydroxide or the aqueous solution of potassium hydroxide.
11. the preparation method of barium titanate-nickel zinc ferrite composite ceramic material according to claim 3, is characterized in that, the described time that reacts completely is 4 hours～6 hours.
12. the preparation method of barium titanate-nickel zinc ferrite composite ceramic material according to claim 3, is characterized in that, described tackiness agent is the aqueous solution of polyvinyl alcohol, and the mass ratio of polyvinyl alcohol and water is 6:100～8:100.
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