CN107638851A - One kind is rung a bell shape Fe3O4@void@SiO2Nano chain and preparation method - Google Patents

One kind is rung a bell shape Fe3O4@void@SiO2Nano chain and preparation method Download PDF

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CN107638851A
CN107638851A CN201710774684.4A CN201710774684A CN107638851A CN 107638851 A CN107638851 A CN 107638851A CN 201710774684 A CN201710774684 A CN 201710774684A CN 107638851 A CN107638851 A CN 107638851A
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CN107638851B (en
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张秋禹
乔明涛
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Northwestern Polytechnical University
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Abstract

Rung a bell shape Fe the present invention relates to one kind3O4@void@SiO2Nano chain and preparation method, first, under the inducing action of external magnetic field, magnetic Fe3O4Nano particle carries out assembling arrangement, promotes polymeric shell layer P (DVB MAA) to wrap Fe3O4Nano particle, so as to form core-shell type Fe3O4@P (DVB MAA) nano chain；Using sol-gal process, to Fe3O4@P (DVB MAA) nano chain carries out SiO2The cladding of shell, realize bivalve layer Fe3O4@P(DVB‑MAA)@SiO2The preparation of nano chain；Finally, Fe is effectively protected using the recrystallization of salt3O4@P(DVB‑MAA)@SiO2The structure of nano chain, is then pyrolyzed in argon atmosphere, and final product is the shape Fe that rings a bell3O4@void@SiO2Nano chain.Special micro-nano structure imparts the good microwave absorbing property of material, and its minimal reflection penalty values is 45.03dB (13.57GHz), and effective absorption band is up to more than 5.5GHz.The invention of the technology efficiently solves the problem of existing absorbing material absorption band is narrower.

Description

One kind is rung a bell shape Fe3O4@void@SiO2Nano chain and preparation method
Technical field
The invention belongs to field of microwave absorption, and in particular to one kind is rung a bell shape Fe3O4@void@SiO2Nano chain and preparation side Method.
Background technology
With the fast development of microwave and mechanics of communication, the electronic equipment such as mobile communication, computer, household electrical appliance is increasingly general And work to people and life bring great convenience.At the same time, electronic equipment can discharge not in the course of the work The electromagnetic wave of same frequency, the normal operation of other electronic equipments is not only disturbed, certain wound also is caused to the health of the mankind Evil, and different degrees of electromagnetic pollution problem is caused to surrounding environment.The electromagnetic pollution problem that urgent need to resolve currently faces. Electromagnetic wave energy can be changed into heat energy or other forms by microwave absorbing material by magnetic loss and dielectric loss mechanism Energy, electromagenetic wave radiation energy is greatly reduced, can effectively alleviate or even eliminate electromagnetic pollution problem, also therefore be considered as It is a kind of candidate of great potential.
According to microwave absorption mechanism, magnetic material and being compounded with for dielectric material are beneficial to improve microwave absorbing material and air Impedance match, make the dissipation for being immersed in material internal, increasing electromagnetic wave energy that incidence wave is as whole as possible；Meanwhile magnetic Loss and the combination of dielectric loss can further enhance microwave absorption effect.Therefore, in recent years, substantial amounts of research work is main Material composition and structure design around magnetic-dielectric composite material is directed to developing new and effective micro- come what is carried out Ripple absorbing material.Common magnetic material has ferrite, simple substance iron-cobalt-nickel, barium titanate etc., and conventional dielectric material is titanium dioxide Silicon, metal-oxide semiconductor (MOS) (zinc oxide, tin oxide, titanium dioxide, copper sulfide), carbon material (graphene, CNT, nothing Shape carbon), conducting polymer (polypyrrole, polythiophene, polyaniline) etc., using different preparation methods, carry out multiple elements design, obtain A series of new nanometer microwave absorbing material is arrived.It is well known that preferably microwave absorbing material need to be provided simultaneously with strong absorption, The features such as broadband, lightweight, low-density.Although many microwave absorbing materials absorbed by force, material are emerged Absorption width still suffer from certain limitation (≤5.0GHz).
The content of the invention
Technical problems to be solved
The shape Fe in order to avoid the shortcomings of the prior art, present invention proposition one kind is rung a bell3O4@void@SiO2Nano chain and Preparation method, it is to provide a kind of novel broadband domain nano wave-absorbing material.
Technical scheme
One kind is rung a bell shape Fe3O4@void@SiO2Nano chain, it is characterised in that：Kernel is Fe3O4, shell SiO2, both Between be cavity；Wherein：The length of nano chain is 10um~30um, and aperture is 5~23nm, BET specific surface area is 90~ 120m2/ g, BJH pore volume are 0.20~0.22cm3。
One kind prepares the shape Fe that rings a bell3O4@void@SiO2The method of nano chain, it is characterised in that step is as follows：
Step 1, core-shell type Fe3O4The preparation of@P (DVB-MAA) nano chain：By Fe3O4Particle, monomer methacrylic acid MAA, cross-linker divinylbenzene DVB are added in 80~100mL acetonitrile, are made it scattered by ultrasound, are then added initiator, The distillation precipitation polymerization of external magnetic field induction is carried out at 80~85 DEG C of bath temperature, reaction obtains core-shell type after 1~1.5 hour Fe3O4@P (DVB-MAA) nano chain；The Fe3O4The concentration of particle is 0.25g/L~0.40g/L, and the concentration of monomer is 3.0g/ L~3.75g/L, the concentration of crosslinking agent is 0.875g/L~1.0g/L；The dosage of the initiator is that monomer is always used with crosslinking agent 1.5wt%~2.0wt% of amount；
Step 2, bivalve layer Fe3O4@P(DVB-MAA)@SiO2The preparation of nano chain：By core-shell type Fe3O4@P(DVB-MAA) Nano chain is scattered in 80mL ethanol-water mixed solvent, then adds 1.5~2.0mL ammoniacal liquor, and mechanical agitation 1~1.5 is small When, it is well mixed solution；0.09~0.11g silicon source is slowly added dropwise, reacts 5~6 hours at room temperature；After Magnetic Isolation It is freeze-dried, dried solid powder is Fe3O4@P(DVB-MAA)@SiO2Nano chain；The alcohol-water mixing is molten Ethanol in agent:The ratio of water is 9~11；
Step 3, ring a bell shape Fe3O4@void@SiO2The preparation of nano chain：By bivalve layer Fe3O4@P(DVB-MAA)@SiO2Receive Rice chain is scattered in 50~80mL saturated aqueous common salts, and rise temperature is evaporated moisture to 80~85 DEG C；It is full by 60~70 DEG C again Add above-mentioned solution and evaporating water several times with saline solution, obtain mixture；Mixture is placed in tube furnace, in argon atmospher Under the protection enclosed 550~650 DEG C calcined after be cooled to after room temperature and wash away sodium chloride crystal with 80~90 DEG C of deionized water With accessory substance, product is collected using Magneto separate, obtains the shape Fe that rings a bell3O4@void@SiO2Nano chain.
Described initiator is azodiisobutyronitrile AIBN or benzoyl peroxide BPO.
Described silicon source is methyl silicate, tetraethyl orthosilicate, positive silicic acid propyl ester, the one or more of butyl silicate.
The concentration of the ammoniacal liquor is 25%~28%.
The heating rate calcined in described step 3 is 1~2 DEG C/min, and calcination time is 6~8h.
Beneficial effect
One kind proposed by the present invention is rung a bell shape Fe3O4@void@SiO2Nano chain and preparation method, first, in external magnetic field Under inducing action, magnetic Fe3O4Nano particle carries out assembling arrangement, at the same time, distills the generation of precipitation polymerization, promotes to polymerize Thing shell P (DVB-MAA) firmly wraps Fe3O4Nano particle, so as to form core-shell type Fe3O4@P (DVB-MAA) nanometer Chain；Using simple sol-gal process, to Fe3O4@P (DVB-MAA) nano chain carries out SiO2The cladding of shell, realize bivalve layer Fe3O4@P(DVB-MAA)@SiO2The preparation of nano chain；Finally, Fe is effectively protected using the recrystallization of salt3O4@P(DVB- MAA)@SiO2The structure of nano chain, is then pyrolyzed in argon atmosphere, and final product is the shape Fe that rings a bell3O4@void@ SiO2Nano chain.Special micro-nano structure imparts the good microwave absorbing property of material, its minimal reflection penalty values for- 45.03dB (13.57GHz), effective absorption band is up to more than 5.5GHz.The invention of the technology efficiently solves existing suction ripple The problem of material absorption band is narrower.
With existing absorbing material, novel broadband domain of the present invention nano wave-absorbing material has advantages below：
1) the one-dimensional taxis of Electromagnetic heating nano chain and high length-diameter ratio, are electromagnetic wave just as numerous microwave antenna Transmission provide directed access, and extend transmission time, be advantageous to the dissipation of electromagnetic energy；
2) nano chain self assembly easily forms tridimensional network, make electromagnetic wave material internal occur Multiple Scattering with repeatedly Absorb, add the waste of electromagnetic wave；
3) substantial amounts of lar nanometric cavities are introduced by shape structure design of ringing a bell, not only reduces the quality of material, additionally it is possible to strengthen The multiple reflections of electromagnetic wave in the cavities are with repeatedly absorbing；
4) special structure imparts the outstanding microwave absorbing property of material, when coating layer thickness is 3.1mm, obtains most strong Reflection loss value -45.03dB (13.57GHz), when coating layer thickness is between 2.9-3.3mm, absorbs width and be all higher than 5.5GHz.
Brief description of the drawings
Fig. 1 is core-shell type Fe3O4The SEM figures and TEM of@P (DVB-MAA) nano chain scheme；
Fig. 2 is bivalve layer Fe3O4@P(DVB-MAA)@SiO2SEM figures and the TEM of nano chain scheme；
Fig. 3 is the shape Fe that rings a bell3O4@void@SiO2SEM figures and the TEM of nano chain scheme；
Fig. 4 is the reflection loss curve of wide frequency domain nano wave-absorbing material；
Fig. 5 is the absorption band width of wide frequency domain nano wave-absorbing material；
Embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described：
Embodiment 1
Step 1, core-shell type Fe3O4The preparation of@P (DVB-MAA) nano chain：By 0.028g Fe3O4The list of particle, 0.26g Body methacrylic acid MAA, 0.08g cross-linker divinylbenzene DVB are added in 80mL acetonitrile, it is uniformly divided by ultrasound Dissipate, then add the initiator azodiisobutyronitrile (AIBN) for accounting for monomer and crosslinking agent total amount 1.6wt%, in 80 DEG C of bath temperature The lower distillation precipitation polymerization for carrying out external magnetic field induction, reaction obtain core-shell type Fe after 1 hour3O4@P (DVB-MAA) nano chain；
Step 2, bivalve layer Fe3O4@P(DVB-MAA)@SiO2The preparation of nano chain：By core-shell type Fe3O4@P(DVB-MAA) Nano chain is scattered in the in the mixed solvent of 73mL ethanol and 7mL water,；Then 1.8mL 25% ammoniacal liquor is added, mechanical agitation 1 is small When, it is well mixed solution；0.09g tetraethyl orthosilicate is slowly added dropwise, reacts 5 hours at room temperature；It is laggard by Magnetic Isolation Row freeze-drying, dried solid powder is Fe3O4@P(DVB-MAA)@SiO2Nano chain；
Step 3, ring a bell shape Fe3O4@void@SiO2The preparation of nano chain：By bivalve layer Fe3O4@P(DVB-MAA)@SiO2Receive Rice chain is scattered in 60mL saturated aqueous common salts, and rise temperature makes moisture slowly be evaporated to 80~85 DEG C；It is full by 60~70 DEG C again Add above-mentioned solution and evaporating water several times with saline solution, obtain mixture；Mixture is placed in tube furnace, in argon atmospher Under the protection enclosed, temperature is risen to 650 DEG C from room temperature with 2 DEG C/min heating rate, calcines 7.5h, be cooled to after room temperature with 80 ~90 DEG C of deionized water washes away sodium chloride crystal and accessory substance, collects product using Magneto separate, obtains the shape Fe that rings a bell3O4@ void@SiO2Nano chain.
Fig. 1 is core-shell type Fe prepared by the embodiment of the present invention 13O4The SEM figures and TEM of@P (DVB-MAA) nano chain scheme, from The length that Fig. 1 can be seen that the nano chain in embodiment 1 is 10~30um, P (DVB-MAA) shell thickness is about 15~ 20nm。
Fig. 2 is bivalve layer Fe prepared by the embodiment of the present invention 13O4@P(DVB-MAA)@SiO2The SEM figures and TEM of nano chain Figure, from figure 2 it can be seen that the shell thickness of nano chain increases 70~80nm.
Fig. 3 is the shape Fe that rings a bell prepared by the embodiment of the present invention 13O4@void@SiO2SEM figures and the TEM of nano chain scheme, from figure As can be seen that kernel is porous magnetic Fe in 33O4Microballoon, outer shell are SiO2, substantial amounts of lar nanometric cavities are left in centre.
Fig. 4 and Fig. 5 is the shape Fe that rings a bell prepared by the embodiment of the present invention 13O4@void@SiO2The reflection loss curve of nano chain With effective absorption band width.
Embodiment 2
Step 1, core-shell type Fe3O4The preparation of@P (DVB-MAA) nano chain：By 0.3g Fe3O4The monomer of particle, 0.3g Methacrylic acid MAA, 0.09g cross-linker divinylbenzene DVB are added in 100mL acetonitrile, it is uniformly divided by ultrasound Dissipate, then add the initiator azodiisobutyronitrile (AIBN) for accounting for monomer and crosslinking agent total amount 1.9wt%, in 85 DEG C of bath temperature The lower distillation precipitation polymerization for carrying out external magnetic field induction, reaction obtain core-shell type Fe after 1.5 hours3O4@P (DVB-MAA) nanometer Chain；
Step 2, bivalve layer Fe3O4@P(DVB-MAA)@SiO2The preparation of nano chain：By core-shell type Fe3O4@P(DVB-MAA) Nano chain is scattered in the in the mixed solvent of 72mL ethanol and 8mL water；Then 1.6mL 28% ammoniacal liquor is added, mechanical agitation 1.5 is small When, it is well mixed solution；0.1g methyl silicate is slowly added dropwise, reacts 6 hours at room temperature；By being carried out after Magnetic Isolation Freeze-drying, dried solid powder is Fe3O4@P(DVB-MAA)@SiO2Nano chain；
Step 3, ring a bell shape Fe3O4@void@SiO2The preparation of nano chain：By bivalve layer Fe3O4@P(DVB-MAA)@SiO2Receive Rice chain is scattered in 70mL saturated aqueous common salts, and rise temperature makes moisture slowly be evaporated to 80~85 DEG C；It is full by 60~70 DEG C again Add above-mentioned solution and evaporating water several times with saline solution, obtain mixture；Mixture is placed in tube furnace, in argon atmospher Under the protection enclosed, temperature is risen to 600 DEG C from room temperature with 1 DEG C/min heating rate, calcines 6h, be cooled to after room temperature with 80~ 90 DEG C of deionized water washes away sodium chloride crystal and accessory substance, collects product using Magneto separate, obtains the shape Fe that rings a bell3O4@void@ SiO2Nano chain.
Embodiment 3
Step 1, core-shell type Fe3O4The preparation of@P (DVB-MAA) nano chain：By 0.026g Fe3O4The list of particle, 0.3g Body methacrylic acid MAA, 0.08g cross-linker divinylbenzene DVB are added in 90mL acetonitrile, it is uniformly divided by ultrasound Dissipate, then add the initiator benzoyl peroxide (BPO) for accounting for monomer and crosslinking agent total amount 1.6wt%, in 80 DEG C of bath temperature The lower distillation precipitation polymerization for carrying out external magnetic field induction, reaction obtain core-shell type Fe after 1 hour3O4@P (DVB-MAA) nano chain；
Step 2, bivalve layer Fe3O4@P(DVB-MAA)@SiO2The preparation of nano chain：By core-shell type Fe3O4@P(DVB-MAA) Nano chain is scattered in the in the mixed solvent of 72mL ethanol and 8mL water；Then 2.0mL 28% ammoniacal liquor is added, mechanical agitation 1.5 is small When, it is well mixed solution；0.11g tetraethyl orthosilicate is slowly added dropwise, reacts 6 hours at room temperature；It is laggard by Magnetic Isolation Row freeze-drying, dried solid powder is Fe3O4@P(DVB-MAA)@SiO2Nano chain；
Step 3, ring a bell shape Fe3O4@void@SiO2The preparation of nano chain：By bivalve layer Fe3O4@P(DVB-MAA)@SiO2Receive Rice chain is scattered in 80mL saturated aqueous common salts, and rise temperature makes moisture slowly be evaporated to 80~85 DEG C；It is full by 60~70 DEG C again Add above-mentioned solution and evaporating water several times with saline solution, obtain mixture；Mixture is placed in tube furnace, in argon atmospher Under the protection enclosed, temperature is risen to 550 DEG C from room temperature with 2 DEG C/min heating rate, calcines 8h, be cooled to after room temperature with 80~ 90 DEG C of deionized water washes away sodium chloride crystal and accessory substance, collects product using Magneto separate, obtains the shape Fe that rings a bell3O4@void@ SiO2Nano chain.
Embodiment 4
Step 1, core-shell type Fe3O4The preparation of@P (DVB-MAA) nano chain：By 0.3g Fe3O4The monomer of particle, 0.28g Methacrylic acid MAA, 0.07g cross-linker divinylbenzene DVB are added in 80mL acetonitrile, it is uniformly divided by ultrasound Dissipate, then add the initiator azodiisobutyronitrile (AIBN) for accounting for monomer and crosslinking agent total amount 1.6wt%, in 85 DEG C of bath temperature The lower distillation precipitation polymerization for carrying out external magnetic field induction, reaction obtain core-shell type Fe after 1.5 hours3O4@P (DVB-MAA) nanometer Chain；
Step 2, bivalve layer Fe3O4@P(DVB-MAA)@SiO2The preparation of nano chain：By core-shell type Fe3O4@P(DVB-MAA) Nano chain is scattered in the in the mixed solvent of 73mL ethanol and 7mL water；Then 2.0mL 25% ammoniacal liquor is added, mechanical agitation 1.5 is small When, it is well mixed solution；0.09g methyl silicate is slowly added dropwise, reacts 6 hours at room temperature；It is laggard by Magnetic Isolation Row freeze-drying, dried solid powder is Fe3O4@P(DVB-MAA)@SiO2Nano chain；
Step 3, ring a bell shape Fe3O4@void@SiO2The preparation of nano chain：By bivalve layer Fe3O4@P(DVB-MAA)@SiO2Receive Rice chain is scattered in 60mL saturated aqueous common salts, and rise temperature makes moisture slowly be evaporated to 80~85 DEG C；It is full by 60~70 DEG C again Add above-mentioned solution and evaporating water several times with saline solution, obtain mixture；Mixture is placed in tube furnace, in argon atmospher Under the protection enclosed, temperature is risen to 600 DEG C from room temperature with 2 DEG C/min heating rate, calcines 6h, be cooled to after room temperature with 80~ 90 DEG C of deionized water washes away sodium chloride crystal and accessory substance, collects product using Magneto separate, obtains the shape Fe that rings a bell3O4@void@ SiO2Nano chain.
Embodiment 5
Step 1, core-shell type Fe3O4The preparation of@P (DVB-MAA) nano chain：By 0.028g Fe3O4The list of particle, 0.3g Body methacrylic acid MAA, 0.09g cross-linker divinylbenzene DVB are added in 100mL acetonitrile, make its uniform by ultrasound It is scattered, the initiator azodiisobutyronitrile (AIBN) for accounting for monomer and crosslinking agent total amount 1.7wt% is then added, in bath temperature 85 The distillation precipitation polymerization of external magnetic field induction is carried out at DEG C, reaction obtains core-shell type Fe after 1 hour3O4@P (DVB-MAA) nanometer Chain；
Step 2, bivalve layer Fe3O4@P(DVB-MAA)@SiO2The preparation of nano chain：By core-shell type Fe3O4@P(DVB-MAA) Nano chain is scattered in the in the mixed solvent of 72mL ethanol and 8mL water；Then 1.8mL 25% ammoniacal liquor is added, mechanical agitation 1 is small When, it is well mixed solution；0.11g butyl silicate is slowly added dropwise, reacts 6 hours at room temperature；It is laggard by Magnetic Isolation Row freeze-drying, dried solid powder is Fe3O4@P(DVB-MAA)@SiO2Nano chain；
Step 3, ring a bell shape Fe3O4@void@SiO2The preparation of nano chain：By bivalve layer Fe3O4@P(DVB-MAA)@SiO2Receive Rice chain is scattered in 80mL saturated aqueous common salts, and rise temperature makes moisture slowly be evaporated to 80~85 DEG C；It is full by 60~70 DEG C again Add above-mentioned solution and evaporating water several times with saline solution, obtain mixture；Mixture is placed in tube furnace, in argon atmospher Under the protection enclosed, temperature is risen to 600 DEG C from room temperature with 1 DEG C/min heating rate, calcines 7h, be cooled to after room temperature with 80~ 90 DEG C of deionized water washes away sodium chloride crystal and accessory substance, collects product using Magneto separate, obtains the shape Fe that rings a bell3O4@void@ SiO2Nano chain.
Embodiment 6
Step 1, core-shell type Fe3O4The preparation of@P (DVB-MAA) nano chain：By 0.3g Fe3O4The monomer of particle, 0.32g Methacrylic acid MAA, 0.08g cross-linker divinylbenzene DVB are added in 100mL acetonitrile, it is uniformly divided by ultrasound Dissipate, then add the initiator azodiisobutyronitrile (AIBN) for accounting for monomer and crosslinking agent total amount 1.8wt%, in 85 DEG C of bath temperature The lower distillation precipitation polymerization for carrying out external magnetic field induction, reaction obtain core-shell type Fe after 1.5 hours3O4@P (DVB-MAA) nanometer Chain；
Step 2, bivalve layer Fe3O4@P(DVB-MAA)@SiO2The preparation of nano chain：By core-shell type Fe3O4@P(DVB-MAA) Nano chain is scattered in the in the mixed solvent of 72.5mL ethanol and 7.5mL water；Then 1.5mL 28% ammoniacal liquor, mechanical agitation 1 are added Hour, it is well mixed solution；0.09g tetraethyl orthosilicate is slowly added dropwise, reacts 5 hours at room temperature；After Magnetic Isolation It is freeze-dried, dried solid powder is Fe3O4@P(DVB-MAA)@SiO2Nano chain；
Step 3, ring a bell shape Fe3O4@void@SiO2The preparation of nano chain：By bivalve layer Fe3O4@P(DVB-MAA)@SiO2Receive Rice chain is scattered in 80mL saturated aqueous common salts, and rise temperature makes moisture slowly be evaporated to 80~85 DEG C；It is full by 60~70 DEG C again Add above-mentioned solution and evaporating water several times with saline solution, obtain mixture；Mixture is placed in tube furnace, in argon atmospher Under the protection enclosed, temperature is risen to 600 DEG C from room temperature with 1 DEG C/min heating rate, calcines 8h, be cooled to after room temperature with 80~ 90 DEG C of deionized water washes away sodium chloride crystal and accessory substance, collects product using Magneto separate, obtains the shape Fe that rings a bell3O4@void@ SiO2Nano chain.

Claims (6)

  1. The shape Fe 1. one kind is rung a bell3O4@void@SiO2Nano chain, it is characterised in that：Kernel is Fe3O4, shell SiO2, both it Between be cavity；Wherein：The length of nano chain is 10um~30um, and aperture is 5~23nm, and BET specific surface area is 90~120m2/ G, BJH pore volume are 0.20~0.22cm3。
  2. 2. one kind prepares the shape Fe that rung a bell described in claim 13O4@void@SiO2The method of nano chain, it is characterised in that step is such as Under：
    Step 1, core-shell type Fe3O4The preparation of@P (DVB-MAA) nano chain：By Fe3O4Particle, monomer methacrylic acid MAA, crosslinking Agent divinylbenzene DVB is added in 80~100mL acetonitrile, is made it scattered by ultrasound, initiator is then added, in water-bath temperature The distillation precipitation polymerization of external magnetic field induction is carried out at 80~85 DEG C of degree, reaction obtains core-shell type Fe after 1~1.5 hour3O4@P (DVB-MAA) nano chain；The Fe3O4The concentration of particle is 0.25g/L~0.40g/L, the concentration of monomer for 3.0g/L~ 3.75g/L, the concentration of crosslinking agent is 0.875g/L~1.0g/L；The dosage of the initiator is monomer and the total dosage of crosslinking agent 1.5wt%~2.0wt%；
    Step 2, bivalve layer Fe3O4@P(DVB-MAA)@SiO2The preparation of nano chain：By core-shell type Fe3O4@P (DVB-MAA) nanometer Chain is scattered in 80mL ethanol-water mixed solvent, then 1.5~2.0mL of addition ammoniacal liquor, mechanical agitation 1~1.5 hour, It is well mixed solution；0.09~0.11g silicon source is slowly added dropwise, reacts 5~6 hours at room temperature；It is laggard by Magnetic Isolation Row freeze-drying, dried solid powder is Fe3O4@P(DVB-MAA)@SiO2Nano chain；The ethanol-water mixed solvent Middle ethanol:The ratio of water is 9~11；
    Step 3, ring a bell shape Fe3O4@void@SiO2The preparation of nano chain：By bivalve layer Fe3O4@P(DVB-MAA)@SiO2Nano chain It is scattered in 50~80mL saturated aqueous common salts, rise temperature is evaporated moisture to 80~85 DEG C；60~70 DEG C of saturation is eaten again Salt solution adds above-mentioned solution and evaporating water several times, obtains mixture；Mixture is placed in tube furnace, in argon atmosphere Lower 550~650 DEG C of protection is cooled to after room temperature after being calcined and washes away sodium chloride crystal and pair with 80~90 DEG C of deionized water Product, product is collected using Magneto separate, obtains the shape Fe that rings a bell3O4@void@SiO2Nano chain.
  3. 3. according to the method for claim 2, it is characterised in that：Described initiator is azodiisobutyronitrile AIBN or peroxide Change benzoyl BPO.
  4. 4. according to the method for claim 2, it is characterised in that：Described silicon source is methyl silicate, tetraethyl orthosilicate, just The one or more of silicic acid propyl ester, butyl silicate.
  5. 5. according to the method for claim 2, it is characterised in that：The concentration of the ammoniacal liquor is 25%~28%.
  6. 6. according to the method for claim 2, it is characterised in that：The heating rate calcined in described step 3 be 1~2 DEG C/ Min, calcination time are 6~8h.
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CN110255536A (en) * 2019-06-24 2019-09-20 王坤 Composite material and preparation method with absorbing property and electromagnetic shielding performance
CN112717843A (en) * 2020-12-07 2021-04-30 安徽师范大学 Tin dioxide quantum dot/carbon nanotube/sulfur particle porous microcapsule composite material and preparation method and application thereof
CN113020586A (en) * 2021-01-19 2021-06-25 武汉科技大学 Oxidation-resistant FeCo @ SiO2Core-shell structure material and preparation method thereof
CN113355687A (en) * 2021-04-20 2021-09-07 广东石油化工学院 Tin-based bimetallic carbide @ carbon nanochain core-shell structure and preparation method and application thereof
WO2023122841A1 (en) * 2021-12-31 2023-07-06 Pontificia Universidad Católica De Chile Cobalt-based catalyst with nanometric structure for the catalytic hydrogenation of olefinic hydrocarbons and oxygenated aromatic substrates

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101514282A (en) * 2009-03-31 2009-08-26 哈尔滨工程大学 Porous Fe3O4/Fe/SiO2 core-shell nanorod absorbing high-frequency electromagnetic waves and a preparation method
CN102502873A (en) * 2011-09-22 2012-06-20 西北工业大学 Preparation method for one-dimensional magnetic nanochain
CN103157430A (en) * 2011-12-09 2013-06-19 中国科学院大连化学物理研究所 Sea-urchin-shaped core-shell type Fe3O4@TiO2 magnetic microspheres, and preparation and application thereof
CN105126715A (en) * 2015-08-29 2015-12-09 复旦大学 Magnetic mesoporous silica microsphere material with yolk structure and preparing method thereof
WO2016085411A1 (en) * 2014-11-25 2016-06-02 Nanyang Technological University Method for preparing a magnetic chain structure
CN106582653A (en) * 2016-11-16 2017-04-26 同济大学 Preparation method of Fe3O4/FeNi nanometer chain-type composite material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101514282A (en) * 2009-03-31 2009-08-26 哈尔滨工程大学 Porous Fe3O4/Fe/SiO2 core-shell nanorod absorbing high-frequency electromagnetic waves and a preparation method
CN102502873A (en) * 2011-09-22 2012-06-20 西北工业大学 Preparation method for one-dimensional magnetic nanochain
CN103157430A (en) * 2011-12-09 2013-06-19 中国科学院大连化学物理研究所 Sea-urchin-shaped core-shell type Fe3O4@TiO2 magnetic microspheres, and preparation and application thereof
WO2016085411A1 (en) * 2014-11-25 2016-06-02 Nanyang Technological University Method for preparing a magnetic chain structure
CN105126715A (en) * 2015-08-29 2015-12-09 复旦大学 Magnetic mesoporous silica microsphere material with yolk structure and preparing method thereof
CN106582653A (en) * 2016-11-16 2017-04-26 同济大学 Preparation method of Fe3O4/FeNi nanometer chain-type composite material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
LE ZHANG 等: "Synthesis and characterization of Fe3O4@SiO2 magnetic composite nanoparticles by a one-pot process", 《INTERNATIONAL JOURNAL OF MINERALS, METALLURGY AND MATERIALS》 *
YONGXING HU 等: "Magnetically Responsive Photonic Nanochains", 《ANGEW. CHEM. INT. ED.》 *

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108147470A (en) * 2018-02-05 2018-06-12 兰州大学 Water solubility stablizes the preparation method of Magnetic guidance photonic crystal
CN108147470B (en) * 2018-02-05 2019-11-05 兰州大学 Water solubility stablizes the preparation method of Magnetic guidance photonic crystal
CN108711480A (en) * 2018-04-03 2018-10-26 复旦大学 One kind having core-shell structure magnetic mesoporous silicon dioxide nano chain and preparation method thereof
CN109935430A (en) * 2019-03-06 2019-06-25 湖南理工学院 A kind of preparation and application of magnetic one-dimensional chain nano-complex
CN110152683A (en) * 2019-05-27 2019-08-23 西北工业大学 One kind can rotation magnetic nano chain supported palladium nano-particle catalyst and preparation method thereof
CN110152683B (en) * 2019-05-27 2022-04-26 西北工业大学 Autorotation magnetic nanochain supported palladium nanoparticle catalyst and preparation method thereof
CN110255536A (en) * 2019-06-24 2019-09-20 王坤 Composite material and preparation method with absorbing property and electromagnetic shielding performance
CN112717843A (en) * 2020-12-07 2021-04-30 安徽师范大学 Tin dioxide quantum dot/carbon nanotube/sulfur particle porous microcapsule composite material and preparation method and application thereof
CN112717843B (en) * 2020-12-07 2022-06-21 安徽师范大学 Tin dioxide quantum dot/carbon nanotube/sulfur particle porous microcapsule composite material and preparation method and application thereof
CN113020586A (en) * 2021-01-19 2021-06-25 武汉科技大学 Oxidation-resistant FeCo @ SiO2Core-shell structure material and preparation method thereof
CN113355687A (en) * 2021-04-20 2021-09-07 广东石油化工学院 Tin-based bimetallic carbide @ carbon nanochain core-shell structure and preparation method and application thereof
WO2023122841A1 (en) * 2021-12-31 2023-07-06 Pontificia Universidad Católica De Chile Cobalt-based catalyst with nanometric structure for the catalytic hydrogenation of olefinic hydrocarbons and oxygenated aromatic substrates

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