CN105668652A - Carbon/nickel-zinc ferrite electromagnetic wave absorbent and preparation method thereof - Google Patents
Carbon/nickel-zinc ferrite electromagnetic wave absorbent and preparation method thereof Download PDFInfo
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- CN105668652A CN105668652A CN201610029705.5A CN201610029705A CN105668652A CN 105668652 A CN105668652 A CN 105668652A CN 201610029705 A CN201610029705 A CN 201610029705A CN 105668652 A CN105668652 A CN 105668652A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- H—ELECTRICITY
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Abstract
The invention discloses a carbon/nickel-zinc ferrite electromagnetic wave absorbent and a preparation method thereof, and belongs to the field of a magnetic function material. The method comprises three main processes: (1) preparation of wood powder/nickel-zinc ferrite precursor xerogel, (2) low temperature pre-burning of the xerogel, and (3) high temperature calcination of a sample under an atmosphere of argon gas. The wood powder has the characteristics of multihole and light weight, the ferrite precursor xerogel is loaded on the surface, low temperature pre-burning of the precursor xerogel is carried out, high temperature calcination is carried out under the atmosphere of argon gas, the wood powder is not completely oxidized, parts of the wood powder are reduced to charcoal, and the carbon/nickel-zinc ferrite electromagnetic wave absorbent is obtained. The microwave absorbent is light, and has dielectric loss and magnetic loss for electromagnetic wave simultaneously.
Description
Technical field
The present invention relates to a kind of charcoal/nickel-zinc ferrite wave absorbing agent, be specifically related to a kind of low-density charcoal/nickel-zinc ferrite wave absorbing agent and preparation method thereof, belong to magnetic functional material field.
Background technology
Ferrite is the absorbing material that research is more also more ripe, and the polarity effect to the existing dielectric property aspect of electromagnetic absorption has again magnetic loss effect. But there is the shortcoming that density is big in ferrite so that its application is restricted.
The problem big in order to solve Ferrite Material density, mainly carries out multicomponent Composite to it both at home and abroad and village hollowing processes. The C microsphere that claret-red virtue (CN102531562A) is prepared using hydro-thermal method, as template, prepares nickel-zinc ferrite-C predecessor complex microsphere, removes template by calcining, obtains the soft magnetism mesoporous nickel Zn ferrite of saturation magnetization up to 85mu/g. An Yuliang (CN102134470A) prepares porous carbon material load nanometer ferrite absorbing material, obtains grain crystalline tiny, does not reunite, and the porous carbon material load iron oxysome ratio being firmly combined with is stronger. Lin Shuai (chemical analysis metering 1008-6145.2014.05.028) prepares Fe by hydro-thermal method3O4/ graphene composite material, when matching thickness is 7mm, composite has two absworption peaks: at 5.5GHz place, absworption peak is-9.5dB, maximum absorption band-36dB occurs at 16.5GHz place.
But the method preparing nickel-zinc ferrite at present is primarily present following defect: relatively costly, complex process, it is unsuitable for the shortcomings such as industrialized production.
Summary of the invention
For solving the defect in existing research, the present invention provides a kind of charcoal/nickel-zinc ferrite wave absorbing agent and preparation method thereof. The present invention adopts sol-gal process, at wood powder area load nickel-zinc ferrite presoma, and high-temperature calcination makes wood powder partially carbonized under argon gas atmosphere, prepare porous charcoal/nickel-zinc ferrite wave absorbing agent, realize composite broadband, the strong characteristic absorbed by cooperative effect.
A kind of charcoal/nickel-zinc ferrite wave absorbing agent preparation method, comprises the following steps:
(1) pretreatment of wood powder: adopting mass percent is the silane coupler solution of 0.5%～10% wood powder surface treatment 10～15min to 40～80 orders, is then dried to over dry at 80～110 DEG C;
(2) preparation of precursor liquid: at room temperature, by Ni0.5Zn0.5Fe2O4In the molal weight of each metallic element weigh the slaine of Ni, Zn and Fe, be dissolved separately in water, obtaining concentration is 0.3mol/L～0.6mol/L mixing salt solution;Adding citric acid in mixed salt solution, stir, the amount adding citric acid is 1:1～1:2 with metal ion mol ratio; To mixed solution and dripping ammonia, regulate pH value of solution to 6～8;
(3) preparation of wood powder base nickel-zinc ferrite xerogel: the mass ratio adding the wood powder of pretreatment, wood powder and metal ion in the solution obtained in step (2) is 1:1～2:1; Being placed in by mixed solution at 60～80 DEG C of temperature, stir 3～6h under 300～600r/mn speed, obtain colloidal sol, be transferred in crucible by colloidal sol, at 100～110 DEG C, dry 24～48h, obtains wood powder/nickel-zinc ferrite xerogel;
(4) formation of porous light nickel-zinc ferrite: by xerogel with the ramp of 4～6 DEG C/min to 400～500 DEG C of pre-burning 2h, cool to room temperature with the furnace, obtain dendroid sample; Dendroid sample is ground into powder, it is warmed up to 800～1000 DEG C with the heating rate of 10～15 DEG C/min under an argon atmosphere, and is incubated 2～3h, after furnace cooling, namely obtain microwave absorption.
Wherein, wood powder one in Poplar Powder, pine powder, fir powder; Described silane coupler one in 3-glycidyl ether oxygen propyl trimethoxy silicane (KH-560), 3-aminopropyl triethoxysilane (KH550). Described slaine one in nitrate, villaumite and sulfate. The present invention also protects the wave absorbing agent prepared according to the method described above.
It is cheap that the present invention has the advantage that wood powder used by the present invention has compared to existing technology, and raw material is feature widely; The present invention, with the wood powder of porous for template, is prepared for the charcoal/nickel-zinc ferrite with loose structure so that ferritic proportion significantly reduces, and bulk density is only 1～3g/cm3, there is the feature of light weight; Wood powder of the present invention, through high temperature cabonization, and can improve its electromagnetic performance after ferrite compound; Microwave absorption of the present invention is with electrical loss characteristic and magnetic loss characteristic.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the charcoal/nickel-zinc ferrite of embodiment 1 preparation;
Fig. 2 is the electromagnetic parameter figure of embodiment 1 charcoal/nickel-zinc ferrite;
Fig. 3 is the electromagnetic parameter figure of embodiment 2 charcoals/nickel-zinc ferrite;
Fig. 4 is the electromagnetic parameter figure of embodiment 3 charcoals/nickel-zinc ferrite;
Fig. 5 is the electromagnetic parameter figure of embodiment 4 charcoals/nickel-zinc ferrite;
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1:
Preparation method is as follows:
(1) pretreatment of wood powder: adopting mass percent is the KH550 silane coupler solution of the 0.5% Poplar Powder surface treatment 10min to 40 orders, is then dried to over dry at 80 DEG C;
(2) preparation of precursor liquid: at room temperature, weighs 4.3622gNi (NO3)2·6H2O、4.4624gZn(NO3)2·6H2O and 24.24gFe (NO3)3·9H2O, is dissolved in 100mL water, prepares metal salt solution; Weigh 18.9126g citric acid and join in metal salt solution, magnetic agitation Homogeneous phase mixing; To mixed solution and dripping ammonia, regulate pH value to 6;
(3) preparation of wood powder base nickel-zinc ferrite xerogel: adding the wood powder 5.1g of pretreatment, 80 DEG C of stirring in water bath 3h in the solution obtained in step (2), mixing speed is 300r/min, obtains colloidal sol; Being transferred in crucible by colloidal sol, at 110 DEG C, dry 24h, obtains wood powder/ferrite presoma xerogel;
(4) formation of porous light charcoal/nickel-zinc ferrite: by the presoma xerogel ramp to 400 DEG C with 4 DEG C/min, pre-burning 2h, then cool to room temperature with the furnace;Dendroid presoma pre-burning obtained is ground into powder, and is placed in tube type vacuum stove, rises to 800 DEG C of insulation 2h with the speed of 10 DEG C/min under an argon atmosphere, is then down to room temperature with stove, obtains cavernous charcoal/nickel-zinc ferrite powder.
Prepared wave absorbing agent powder X-ray diffractometer (XRD) is carried out material phase analysis, as shown in Fig. 1 (a), the position of result display main diffraction peak is strong with peak all corresponding with nickel-zinc ferrite crystal, illustrates to obtain the nickel-zinc ferrite of spinel-type.
Prepared wave absorbing agent powder is carried out electromagnetic parameter testing, as in figure 2 it is shown, have good electromagnetic parameter within the scope of 0.1-18GHz.
Embodiment 2:
Preparation method is as follows:
(1) pretreatment of wood powder: adopting mass percent is the KH560 silane coupler solution of the 3% Poplar Powder surface treatment 12min to 60 orders, is then dried to over dry at 90 DEG C;
(2) preparation of precursor liquid: at room temperature, weigh 3.56gNiCl2·6H2O、2.04gZnCl2And 16.2gFeCl3·6H2O, is dissolved in 100mL water, prepares metal salt solution; Weigh 31.521g citric acid and join in metal salt solution, magnetic agitation Homogeneous phase mixing; To mixed solution and dripping ammonia, regulate pH value to 6.5;
(3) preparation of wood powder base nickel-zinc ferrite xerogel: adding the wood powder 11.73g of pretreatment, 70 DEG C of stirring in water bath 4h in the solution obtained in step (2), mixing speed is 400r/min, obtains colloidal sol; Being transferred in crucible by colloidal sol, at 105 DEG C, dry 30h, obtains wood powder/ferrite presoma xerogel;
(4) formation of porous light charcoal/nickel-zinc ferrite: presoma xerogel is raised to 500 DEG C with the speed of 5 DEG C/min, pre-burning 2h, then cool to room temperature with the furnace; Dendroid presoma is ground into powder, is placed in tube type vacuum stove, rise to 900 DEG C of insulation 3h with the speed of 12 DEG C/min under an argon atmosphere, cool to room temperature with the furnace, obtain cavernous charcoal/nickel-zinc ferrite powder.
Prepared wave absorbing agent powder X-ray diffractometer (XRD) is carried out material phase analysis, as shown in Fig. 1 (b), the position of result display main diffraction peak is strong with peak all corresponding with nickel-zinc ferrite crystal, illustrates to obtain the nickel-zinc ferrite of spinel-type.
Prepared wave absorbing agent powder is carried out electromagnetic parameter testing, there is within the scope of 0.1-18GHz good electromagnetic parameter.
Embodiment 3:
Preparation method is as follows:
(1) pretreatment of wood powder: adopting mass percent is the KH560 silane coupler solution of the 5% pine powder surface treatment 15min to 70 orders, is then dried to over dry at 100 DEG C;
(2) preparation of precursor liquid: at room temperature, weigh 1.31gNiSO4·6H2O、1.4gZnSO4·7H2O and 8gFe2(SO4)3·9H2O, is dissolved in 100mL water, prepares mixed salt solution; Weigh 13g citric acid and join in metal salt solution, magnetic agitation Homogeneous phase mixing; To mixed solution and dripping ammonia, regulate pH value to 7;
(3) preparation of wood powder base nickel-zinc ferrite xerogel: add the wood powder 4.6938g of pretreatment in the solution obtained in step (2), 80 DEG C of stirring in water bath 4h, mixing speed is 600r/min, obtain colloidal sol, colloidal sol is transferred in crucible, at 110 DEG C, dry 32h, obtains wood powder/nickel-zinc ferrite presoma xerogel;
(4) formation of porous light charcoal/nickel-zinc ferrite: presoma xerogel is raised to 500 DEG C with the speed of 6 DEG C/min, pre-burning 2h, then cool to room temperature with the furnace; By dendroid precursor grinds powder, being placed in tube type vacuum stove, the speed of 15 DEG C/min rises to 1000 DEG C of insulation 2h under an argon atmosphere, is down to room temperature with stove, obtains cavernous charcoal/nickel-zinc ferrite powder.
Prepared wave absorbing agent powder X-ray diffractometer (XRD) is carried out material phase analysis, as shown in Fig. 1 (c), the position of result display main diffraction peak is strong with peak all corresponding with nickel-zinc ferrite crystal, illustrates to obtain the nickel-zinc ferrite of spinel-type.
Prepared wave absorbing agent powder is carried out electromagnetic parameter testing, there is within the scope of 0.1-18GHz good electromagnetic parameter.
Embodiment 4:
Preparation method is as follows:
(1) pretreatment of wood powder: adopting mass percent is the KH550 silane coupler solution of the 8% fir powder surface treatment 14min to 80 orders, is then dried to over dry at 110 DEG C;
(2) preparation of precursor liquid: at room temperature, weighs 32.32gFe (NO3)3·9H2O and 5.9498gZn (NO3)2·6H2O、5.8162gNi(NO3)2·6H2O, is dissolved in 200mL water, prepares mixed salt solution; Weigh 25.2168g citric acid and join in metal salt solution, magnetic agitation Homogeneous phase mixing; To mixed solution and dripping ammonia, regulate pH value to 8;
(3) preparation of wood powder base nickel-zinc ferrite xerogel: add the wood powder 9.3876g of pretreatment, 60 DEG C of stirring in water bath 5h, mixing speed 500r/min in the solution obtained in step (2), obtain colloidal sol; Being transferred in crucible by colloidal sol, at 105 DEG C, dry 48h, obtains wood powder/nickel-zinc ferrite presoma xerogel;
(4) formation of porous light charcoal/nickel-zinc ferrite: presoma xerogel is placed in Muffle furnace and is raised to 500 DEG C with the speed of 6 DEG C/min, pre-burning 2h, then cool to room temperature with the furnace; Dendroid precursor grinds powder pre-burning obtained, is placed in tube type vacuum stove, rises to 1000 DEG C of insulation 3h with the speed of 13 DEG C/min under an argon atmosphere, is down to room temperature with stove, obtains cavernous charcoal/nickel-zinc ferrite powder.
Prepared wave absorbing agent powder X-ray diffractometer (XRD) is carried out material phase analysis, as shown in Fig. 1 (d), the position of result display main diffraction peak is strong with peak all corresponding with nickel-zinc ferrite crystal, and there is no other thing phase peak, illustrate to obtain the nickel-zinc ferrite of spinel-type.
Prepared wave absorbing agent powder is carried out electromagnetic parameter testing, there is within the scope of 0.1-18GHz good electromagnetic parameter.
Claims (5)
1. the preparation method of charcoal/nickel-zinc ferrite wave absorbing agent, it is characterised in that comprise the following steps:
(1) pretreatment of wood powder: adopting mass percent is the silane coupler solution of 0.5%～10% wood powder surface treatment 10～15min to 40～80 orders, is then dried to over dry at 80～110 DEG C;
(2) preparation of precursor liquid: at room temperature, by Ni0.5Zn0.5Fe2O4In the molal weight of each metallic element weigh the slaine of Ni, Zn and Fe, be dissolved separately in water, obtaining concentration is 0.3mol/L～0.6mol/L mixing salt solution; Adding citric acid in mixed salt solution, be uniformly mixing to obtain mixed solution, the amount adding citric acid is 1:1～1:2 with metal ion mol ratio; To mixed solution and dripping ammonia, regulate pH value of solution to 6～8;
(3) preparation of wood powder base nickel-zinc ferrite xerogel: the mass ratio adding the wood powder of pretreatment, wood powder and metal ion in the solution obtained in step (2) is 1:1～2:1; Being placed in by mixed solution at 60～80 DEG C of temperature, stir 3～6h under 300～600r/mn speed, obtain colloidal sol, be transferred in crucible by colloidal sol, at 100～110 DEG C, dry 24～48h, obtains wood powder/nickel-zinc ferrite xerogel;
(4) formation of porous light nickel-zinc ferrite: by xerogel with the ramp of 4～6 DEG C/min to 400～500 DEG C of pre-burning 2h, cool to room temperature with the furnace, obtain dendroid sample;Dendroid sample is ground into powder, it is warmed up to 800～1000 DEG C with the heating rate of 10～15 DEG C/min under an argon atmosphere, and is incubated 2～3h, after furnace cooling, namely obtain microwave absorption.
2. in accordance with the method for claim 1, it is characterised in that described wood powder one in Poplar Powder, pine powder, fir powder.
3. in accordance with the method for claim 1, it is characterised in that described silane coupler one in 3-glycidyl ether oxygen propyl trimethoxy silicane, 3-aminopropyl triethoxysilane.
4. in accordance with the method for claim 1, it is characterised in that the slaine of described step (2) one in nitrate, villaumite and sulfate.
5. the wave absorbing agent prepared by any one method of claim 1-4.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107629624A (en) * | 2017-09-15 | 2018-01-26 | 广州中国科学院工业技术研究院 | Rare earth metal ferroalloy wave absorbing agent and preparation method thereof, application |
| CN110734048A (en) * | 2019-11-18 | 2020-01-31 | 哈尔滨工业大学（威海） | Preparation method of three-dimensional ordered carbon-based porous wave-absorbing material based on raw wood |
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Cited By (3)
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| CN107629624A (en) * | 2017-09-15 | 2018-01-26 | 广州中国科学院工业技术研究院 | Rare earth metal ferroalloy wave absorbing agent and preparation method thereof, application |
| CN107629624B (en) * | 2017-09-15 | 2019-11-26 | 广州中国科学院工业技术研究院 | Rare earth metal ferroalloy wave absorbing agent and preparation method thereof, application |
| CN110734048A (en) * | 2019-11-18 | 2020-01-31 | 哈尔滨工业大学（威海） | Preparation method of three-dimensional ordered carbon-based porous wave-absorbing material based on raw wood |
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