CN105565390B - Diatomite base/nickel-zinc ferrite electromagnetic wave absorber and preparation method thereof - Google Patents
Diatomite base/nickel-zinc ferrite electromagnetic wave absorber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a diatomite base/nickel-zinc ferrite microwave absorber and a preparation method thereof, belonging to the field of magnetic functional materials. The electromagnetic wave absorber takes porous diatomite as a template; the surface of the microwave absorber is adsorbed and coated with NixZn(1-x)Fe2O4 ferrite, the value range of X is 0.3 to 1, and mass percentage of diatomite is 10 to 60 percent. The electromagnetic wave absorber is prepared by adopting a sol-gel method. The ferrite prepared by the invention is light in mass; compared with a preparation process of general ferrite, the preparation process disclosed by the invention has the characteristics that the calcination temperature of the ferrite is lower and the condition that calcination is performed in reducing atmosphere is avoided. The electromagnetic wave absorber disclosed by the invention can be used for protecting electromagnetic radiation of a building. The preparation method disclosed by the invention is simple, convenient in operation and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of magnetic nickel-zinc ferrite wave absorbing agent, and in particular to a kind of low-density diatom soil matrix/nickel zinc iron
Oxysome wave absorbing agent and preparation method thereof, belongs to magnetic functional material field.
Background technology
Spinel-type nickel-zinc ferrite is a kind of important functional magnetic material, because it has high resistivity, low temperature
The features such as coefficient, high-curie temperature, good high frequency performance, in high-frequency inductor magnetic core, transformer, magnetic recording material, microwave absorption
The applications such as material occupy highly important status.But traditional ferrite powder has the shortcomings that density is big, limits it
Using.
Ferritic preparation method is a lot, and conventional has coprecipitation, hydrothermal synthesis method, microemulsion method and sol-gel
Method etc..It is big to solve the problems, such as Ferrite Material density, both at home and abroad Composite is mainly carried out to it and village hollowing is processed.Zhang Yanqing
Citrate Sol-Gel method is utilized Deng (Journal of Inorganic Materials 1000-324X (2009) 04-0732-05), is prepared hollow micro-
Pearl-barium, strontium, cobalt nickel barium ferrite composite granule coating, the microwave reflection loss in 5-18GHz is more than simple ferrite coating;
Gu Yingying (magnetic material and device 1001-3830 (2007) 02-0037-03) adopts hydrothermal template process, with triethylamine and poly- second
Glycol is prepared for density for 4g/cm as template3~4.7g/cm3Nanometer micropore nickel-zinc ferrite;Albuquerque
(277-280 of Journal of Magnetism and Magnetic Materials 192 (1999)) utilizes sol-gal process,
In SiO2Surface coating nickel-zinc ferrite, its saturation magnetization and coercivity are all higher than common nickel-zinc ferrite.Wei generation assistant officer (CN
102531563 A) nickel zinc-magnesium-lanthanum ferrite nano wave-absorbing material is prepared using sol-gal process, it has two in 1-18GHz
Absorb interval, realize that wideband absorbs.Qiu Qin (A of CN 101665635) is precious using cenosphere, perforate expanded perlite and closed pore
Zhu Yan is prepared for certain heat insulation effect for template, and the good ferrite of absorbing property-porous composite granule.An Yuliang (CN
102134470 A) porous carbon material load nanometer ferrite absorbing material is prepared, it is tiny to obtain grain crystalline, does not reunite, and ties
Close firm porous carbon material load ferrite more firm.The red virtue (A of CN 102531562) of wine is micro- with C prepared by hydro-thermal method
Ball prepares nickel-zinc ferrite-C predecessor complex microspheres as template, and by calcining removing template is removed, and obtains saturation magnetization high
Up to the soft magnetism mesopore nickel-zinc ferrite of 85mu/g.
Diatomite main component is amorphous Si O2, greatly, it is mainly used in the original of filter aid, adsorbent and carrier to porosity
Material.Meng Yanyan (A of CN 102513083) is in diatomite particle area load nano zine oxide so that nano zine oxide is to visible
The utilization rate of light and photocatalysis performance are improved.
The method for preparing Ni ferrite at present is primarily present following defect:Hollow template is easily broken, relatively costly, calcining
The shortcomings of temperature height, complex process.
The content of the invention
To solve the deficiencies in the prior art, the present invention provides a kind of diatom soil matrix/nickel-zinc ferrite wave absorbing agent and its preparation
Method.Diatom soil matrix/nickel-zinc ferrite the wave absorbing agent has diatomite for core, shell parcel NiXZn1-XFe2O4Ferritic core
Shell structure, is prepared by sol-gel method, and its preparation method is simple, and cost is relatively low, is suitable to industrial metaplasia
Produce;Prepared diatom soil matrix/nickel-zinc ferrite wave absorbing agent has good magnetic particles.
A kind of diatom soil matrix/nickel-zinc ferrite wave absorbing agent, it is characterised in that:The absorbent is with porous diatomite as base
Body, in its area load NixZn1-xFe2O4The span of ferrite, wherein X is 0.3~1;The diatomaceous quality of the porous
Degree 10%~60%.
A kind of diatom soil matrix/nickel-zinc ferrite wave absorbing agent and preparation method thereof, comprises the following steps:
(1) diatomaceous pretreatment:Diatomite is cleaned into 2h~4h with the hydrochloric acid of 0.1mol/L~0.5mol/L, after filtration
Deionized water is cleaned to neutrality, after filtering it is dried to over dry at 60~100 DEG C, then calcines 2 at 400~460 DEG C of Jing
~4h.
(2) preparation of precursor liquid:At room temperature, by NiXZn1-XFe2O4In each metallic element molal weight (wherein X's
Span is 0.3~slaine of Ni, Zn and Fe 1) is weighed, it is dissolved in water, and concentration is obtained for 0.45~0.9mol/
The mixing salt solution of L;Citric acid is added in mixed salt solution, is stirred, add the amount and metal ion of citric acid
Mol ratio is 1:1~1:2;To mixed solution and dripping ammoniacal liquor, pH value of solution is adjusted to 5~8;
(3) preparation of diatom soil matrix nickel-zinc ferrite xerogel:Diatomite is added in the solution obtained in step (2),
The diatomaceous amount for adding is 1 with the mass ratio of metal ion:2~2:1;By mixed solution 300 at a temperature of 60~90 DEG C~
3~6h is stirred under 600r/min speed, sticky colloidal sol is obtained, colloidal sol is transferred in crucible, in 100~130 DEG C of dryings 20
~40h, obtains diatom soil matrix nickel-zinc ferrite presoma xerogel;
(4) formation of diatom soil matrix nickel-zinc ferrite:By xerogel with the ramp of 4~6 DEG C/min to 210~240
DEG C pre-burning, xerogel forms fluffy dendroid;Dendroid sample is cooled to into grinding at room temperature powdered, by it with heating rate
10~15 DEG C/min is warmed up to 600~900 DEG C, and is incubated 2~4h, and microwave absorption is obtained final product after along with the furnace cooling.
The slaine of the step (2) mainly includes nitrate, villaumite and sulfate.
The present invention has compared to existing technology advantage:The present invention is prepared with the extremely strong diatomite of adsorptivity as template
Diatom soil matrix/Ni Zn ferrimagnet composite material so that the proportion of diatom soil matrix/nickel-zinc ferrite significantly drops compared with pure iron oxysome
Low, density is only 1.5~3g/cm2, the characteristics of with light weight;Diatomite template raw material used of the invention is extensively, cheap;
Microwave absorption of the present invention is with electrical loss characteristic and magnetic loss characteristic.
Description of the drawings
Fig. 1 is the XRD of diatom soil matrix/nickel-zinc ferrite prepared by embodiment 1;
Fig. 2 is the SEM figures before and after the tripolite loading nickel-zinc ferrite of embodiment 1;A () is for load before;B () is for load after
Fig. 3 is the electromagnetic parameter figure of the diatom soil matrix of embodiment 1/nickel-zinc ferrite;
Fig. 4 is the electromagnetic parameter figure of the diatom soil matrix of embodiment 2/nickel-zinc ferrite;
Fig. 5 is the electromagnetic parameter figure of the diatom soil matrix of embodiment 3/nickel-zinc ferrite;
Fig. 6 is the electromagnetic parameter figure of the diatom soil matrix of embodiment 4/nickel-zinc ferrite;
Fig. 7 is the electromagnetic parameter figure of the diatom soil matrix of embodiment 5/nickel-zinc ferrite;
(a) complex dielectric permittivity in wherein Fig. 3-7, (b) complex permeability)
Specific embodiment
Embodiment 1
(1) diatomaceous pretreatment:Diatomite is cleaned into 2h with the hydrochloric acid of 0.1mol/L, deionized water cleaning after filtration
To neutral, it is dried to over dry at 60 DEG C after filtering, then 4h is calcined at 400 DEG C of Jing.
(2) preparation of precursor liquid:Under room temperature, by 2.1384gNiCl2·6H2O、2.8623gZnCl2And 16.2g
FeCl3·6H2O is dissolved in 100mL water and obtains mixed salt solution;18.9126g citric acids are added in mixed solution, is stirred
Mix uniform, to mixed solution and dripping ammoniacal liquor, adjust pH value of solution to 5;
(3) preparation of diatom soil matrix nickel-zinc ferrite xerogel:7.14g silicon is added in the solution obtained in step (2)
Diatomaceous earth, by mixed solution 6h is stirred in 60 DEG C, and mixing speed is 400r/min, obtains sticky colloidal sol, and colloidal sol is transferred to
In crucible, 20h is dried in 100 DEG C, obtains diatom soil matrix nickel-zinc ferrite presoma xerogel;
(4) formation of diatom soil matrix nickel-zinc ferrite:Xerogel is raised to into 210 DEG C by room temperature with the speed of 4 DEG C/min, is protected
Warm 30min, is then down to room temperature with stove;Dendroid sample is cooled to into grinding at room temperature powdered, in being placed Muffle furnace
700 DEG C of insulation 4h are risen to the speed of 10 DEG C/min, diatom soil matrix nickel zinc ferrite microwave absorbent is obtained final product after along with the furnace cooling.
Obtained wave absorbing agent powder is carried out into material phase analysis with X-ray diffractometer (XRD), as shown in figure 1, result shows master
Want the position of diffraction maximum corresponding all with nickel-zinc ferrite crystal with peak intensity, illustrate the Ni ferrite for having obtained spinel-type, remove
There was only diatomaceous SiO outside this2Diffraction maximum.
Obtained absorbent powder ESEM (SEM) is observed into its microstructure, as shown in Fig. 2 result shows institute
Obtained nickel-zinc ferrite is supported on diatom soil pores and its surface.
Obtained wave absorbing agent powder is carried out into electromagnetic parameter testing, as shown in figure 3, having preferably electricity in the range of 0-1GHz
Magnetic parameter.
Embodiment 2
(1) diatomaceous pretreatment:Diatomite is cleaned into 3h with the hydrochloric acid of 0.3mol/L, deionized water cleaning after filtration
To neutral, it is dried to over dry at 80 DEG C after filtering, then 3h is calcined at 420 DEG C of Jing.
(2) preparation of precursor liquid:Under room temperature, by 4.3622gNi (NO3)2·6H2O、4.4624gZn(NO3)2·6H2O and
24.24g Fe(NO3)3·9H2O is dissolved in 100mL deionized waters, obtains mixed salt solution;Add in mixed solution
18.9126g citric acids, stir, and to mixed solution and dripping ammoniacal liquor, adjust pH value of solution to 5;
(3) preparation of diatom soil matrix nickel-zinc ferrite xerogel:6g diatoms are added in the solution obtained in step (2)
Soil, by mixed solution 4h is stirred at a temperature of 70 DEG C, and mixing speed is 300r/min, obtains sticky colloidal sol, and colloidal sol is shifted
Into crucible, 26h is dried in 110 DEG C, obtains diatom soil matrix nickel-zinc ferrite presoma xerogel;
(4) formation of diatom soil matrix nickel-zinc ferrite:Xerogel is raised to into 220 DEG C by room temperature with the speed of 5 DEG C/min, is protected
Warm 30min, is then down to room temperature with stove;Dendroid sample is cooled to into grinding at room temperature powdered, in being placed Muffle furnace
800 DEG C of insulation 2h are risen to the speed of 12 DEG C/min, diatom soil matrix nickel zinc ferrite microwave absorbent is obtained final product after along with the furnace cooling.
Obtained wave absorbing agent powder is carried out into material phase analysis with X-ray diffractometer (XRD), it is as a result similar to Example 1, it is main
Want the position of diffraction maximum corresponding all with nickel-zinc ferrite crystal with peak intensity, illustrate the Ni ferrite for having obtained spinel-type, remove
There was only diatomaceous SiO outside this2Diffraction maximum.
Obtained absorbent powder ESEM (SEM) is observed into its microstructure, as a result similar to Example 1, institute
Obtained nickel-zinc ferrite is supported on diatom soil pores and its surface.
Obtained wave absorbing agent powder is carried out into electromagnetic parameter testing, as shown in figure 4, having preferably electricity in the range of 0-1GHz
Magnetic parameter.
Embodiment 3
(1) diatomaceous pretreatment:Diatomite is cleaned into 4h with the hydrochloric acid of 0.5mol/L, deionized water cleaning after filtration
To neutral, it is dried to over dry at 90 DEG C after filtering, then 2h is calcined at 430 DEG C of Jing.
(2) preparation of precursor liquid:Under room temperature, by 1.9714gNiSO4·6H2O、2.1525gZnSO4·7H2O and
8.4276g Fe2(SO4)3·9H2O is dissolved in 100mL deionized waters, obtains mixed salt solution;Add in mixed solution
18g citric acids, stir, and to mixed solution and dripping ammoniacal liquor, adjust pH value of solution to 6;
(3) preparation of diatom soil matrix nickel-zinc ferrite xerogel:7.14g silicon is added in the solution obtained in step (2)
Diatomaceous earth, by mixed solution 5h is stirred at a temperature of 70 DEG C, and mixing speed is 400r/min, obtains sticky colloidal sol, and colloidal sol is turned
In moving to crucible, 30h is dried in 120 DEG C, obtains diatom soil matrix nickel-zinc ferrite presoma xerogel;
(4) formation of diatom soil matrix nickel-zinc ferrite:Xerogel is raised to into 240 DEG C by room temperature with the speed of 6 DEG C/min, is protected
Warm 30min, is then down to room temperature with stove;Dendroid sample is cooled to into grinding at room temperature powdered, in being placed Muffle furnace
800 DEG C of insulation 3h are risen to the speed of 14 DEG C/min, diatom soil matrix nickel zinc ferrite microwave absorbent is obtained final product after along with the furnace cooling.
Obtained wave absorbing agent powder is carried out into material phase analysis with X-ray diffractometer (XRD), it is as a result similar to Example 1, it is main
Want the position of diffraction maximum corresponding all with nickel-zinc ferrite crystal with peak intensity, illustrate the Ni ferrite for having obtained spinel-type, remove
There was only diatomaceous SiO outside this2Diffraction maximum.
Obtained absorbent powder ESEM (SEM) is observed into its microstructure, as a result similar to Example 1, institute
Obtained nickel-zinc ferrite is supported on diatom soil pores and its surface.
Obtained wave absorbing agent powder is carried out into electromagnetic parameter testing, as shown in figure 5, having preferably electricity in the range of 0-1GHz
Magnetic parameter.
Embodiment 4
(1) diatomaceous pretreatment:Diatomite is cleaned into 2h with the hydrochloric acid of 0.2mol/L, deionized water cleaning after filtration
To neutral, it is dried to over dry at 100 DEG C after filtering, then 3h is calcined at 440 DEG C of Jing.
(2) preparation of precursor liquid:Under room temperature, by 6.107gNi (NO3)2·6H2O、2.6774gZn(NO3)2·6H2O and
24.24g Fe(NO3)3·9H2O is dissolved in 200mL deionized waters, obtains mixed salt solution;Add in mixed solution
20.5g citric acids, stir, and to mixed solution and dripping ammoniacal liquor, adjust pH value of solution to 7;
(3) preparation of diatom soil matrix nickel-zinc ferrite xerogel:3.07g silicon is added in the solution obtained in step (2)
Diatomaceous earth, stirs 4h at a temperature of mixed solution is placed in into 80 DEG C, mixing speed is 500r/min, obtains sticky colloidal sol, by colloidal sol
In being transferred to crucible, 40h is dried in 125 DEG C, obtains diatom soil matrix nickel-zinc ferrite presoma xerogel;
(4) formation of diatom soil matrix nickel-zinc ferrite:Xerogel is raised to into 210 DEG C by room temperature with the speed of 6 DEG C/min, is protected
Warm 30min, is then down to room temperature with stove;Dendroid sample is cooled to into grinding at room temperature powdered, in being placed Muffle furnace
900 DEG C of insulation 3h are risen to the speed of 15 DEG C/min, diatom soil matrix nickel zinc ferrite microwave absorbent is obtained final product after along with the furnace cooling.
Obtained wave absorbing agent powder is carried out into material phase analysis with X-ray diffractometer (XRD), it is as a result similar to Example 1, it is main
Want the position of diffraction maximum corresponding all with nickel-zinc ferrite crystal with peak intensity, illustrate the Ni ferrite for having obtained spinel-type, remove
There was only diatomaceous SiO outside this2Diffraction maximum.
Obtained absorbent powder ESEM (SEM) is observed into its microstructure, as a result similar to Example 1, institute
Obtained nickel-zinc ferrite is supported on diatom soil pores and its surface.
Obtained wave absorbing agent powder is carried out into electromagnetic parameter testing, as shown in fig. 6, having preferably electricity in the range of 0-1GHz
Magnetic parameter.
Embodiment 5
(1) diatomaceous pretreatment:Diatomite is cleaned into 4h with the hydrochloric acid of 0.3mol/L, deionized water cleaning after filtration
To neutral, it is dried to over dry at 100 DEG C after filtering, then 2h is calcined at 450 DEG C of Jing.
(2) preparation of precursor liquid:Under room temperature, by 8.7243g Ni (NO3)2·6H2O、24.24g Fe(NO3)3·9H2O is molten
Solution obtains mixed salt solution in 100mL water;37.8g citric acids are added in mixed solution, is stirred, it is molten to mixing
Ammoniacal liquor is added dropwise in liquid, pH value of solution is adjusted to 8;
(3) preparation of diatom soil matrix nickel-zinc ferrite xerogel:10g diatoms are added in the solution obtained in step (2)
Soil, stirs 3h at a temperature of mixed solution is placed in into 90 DEG C, mixing speed is 500r/min, obtains sticky colloidal sol, and colloidal sol is turned
In moving to crucible, 30h is dried in 130 DEG C, obtains diatom soil matrix nickel-zinc ferrite presoma xerogel;
(4) formation of diatom soil matrix nickel-zinc ferrite:Xerogel is raised to into 230 DEG C in room temperature with the speed of 5 DEG C/min, is protected
Warm 30min, is then down to room temperature with stove;Dendroid sample is cooled to into grinding at room temperature powdered, in being placed Muffle furnace
700 DEG C of insulation 4h are risen to the speed of 13 DEG C/min, diatom soil matrix nickel zinc ferrite microwave absorbent is obtained final product after along with the furnace cooling.
Obtained wave absorbing agent powder is carried out into material phase analysis with X-ray diffractometer (XRD), it is as a result similar to Example 1, it is main
Want the position of diffraction maximum corresponding all with nickel-zinc ferrite crystal with peak intensity, illustrate the Ni ferrite for having obtained spinel-type, remove
There was only diatomaceous SiO outside this2Diffraction maximum.
Obtained absorbent powder ESEM (SEM) is observed into its microstructure, as a result similar to Example 1, institute
Obtained nickel-zinc ferrite is supported on diatom soil pores and its surface.
Obtained wave absorbing agent powder is carried out into electromagnetic parameter testing, as shown in fig. 7, having preferably electricity in the range of 0-1GHz
Magnetic parameter.
Claims (2)
1. a kind of preparation method of diatom soil matrix/nickel-zinc ferrite wave absorbing agent, the absorbent based on porous diatomite,
Its area load NixZn1-xFe2O4The span of ferrite, wherein X is 0.3~1;The diatomaceous quality percentage of the porous
Than content 10%~60%;
Characterized in that, comprising the following steps:
(1) diatomaceous pretreatment:Diatomite is cleaned into 2h~4h with the hydrochloric acid of 0.1mol/L~0.5mol/L, is spent after filtration
Ionized water is cleaned to neutrality, after filtering it is dried to over dry at 60~100 DEG C, then 2~4h is calcined at 400~460 DEG C of Jing;
(2) preparation of precursor liquid:At room temperature, by NiXZn1-XFe2O4In the molal weight of each metallic element weigh Ni, Zn and Fe
Slaine, be dissolved in water, obtain the mixing salt solution that concentration is 0.45~0.9mol/L;The wherein span of X
For 0.3~1;Citric acid is added in mixed salt solution, is stirred, add the amount and metal ion mol ratio of citric acid
For 1:1~1:2;To mixed solution and dripping ammoniacal liquor, pH value of solution is adjusted to 5~8;
(3) preparation of diatom soil matrix nickel-zinc ferrite xerogel:Diatomite is added in the solution obtained in step (2), is added
The mass ratio of diatomaceous amount and metal ion be 1:2~2:1;By mixed solution at a temperature of 60~90 DEG C 300~600r/
3~6h is stirred under min speed, sticky colloidal sol is obtained, colloidal sol is transferred in crucible, in 100~130 DEG C of 20~40h of drying,
Obtain diatom soil matrix nickel-zinc ferrite presoma xerogel;
(4) formation of diatom soil matrix nickel-zinc ferrite:Xerogel is pre- to 210~240 DEG C with the ramp of 4~6 DEG C/min
Burn, xerogel forms fluffy dendroid;Dendroid sample is cooled to into grinding at room temperature powdered, by its with heating rate 10~
15 DEG C/min is warmed up to 600~900 DEG C, and is incubated 2~4h, and microwave absorption is obtained final product after along with the furnace cooling.
2. preparation method according to claim 1, it is characterised in that:
The slaine of step (2) includes nitrate, villaumite or sulfate.
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CN102528886A (en) * | 2010-12-13 | 2012-07-04 | 中国建筑材料科学研究总院 | Composite shaving board with electromagnetic wave absorbing function and manufacturing method of composite shaving board |
CN102773105A (en) * | 2012-08-06 | 2012-11-14 | 河南师范大学 | Supported bismuth tungstate photocatalyst and preparation method thereof |
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US6641908B1 (en) * | 2001-05-18 | 2003-11-04 | Ensci Inc | Metal oxide coated diatomite substrates |
CN102528886A (en) * | 2010-12-13 | 2012-07-04 | 中国建筑材料科学研究总院 | Composite shaving board with electromagnetic wave absorbing function and manufacturing method of composite shaving board |
CN102773105A (en) * | 2012-08-06 | 2012-11-14 | 河南师范大学 | Supported bismuth tungstate photocatalyst and preparation method thereof |
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