CN102965074A - Nanoparticle for absorbing microwave and synthesis method thereof - Google Patents
Nanoparticle for absorbing microwave and synthesis method thereof Download PDFInfo
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- CN102965074A CN102965074A CN2012105058423A CN201210505842A CN102965074A CN 102965074 A CN102965074 A CN 102965074A CN 2012105058423 A CN2012105058423 A CN 2012105058423A CN 201210505842 A CN201210505842 A CN 201210505842A CN 102965074 A CN102965074 A CN 102965074A
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Abstract
The invention provides a nanoparticle for absorbing a microwave and a synthesis method thereof. The nanoparticle comprises a base material which is ferroferric oxide and a shell layer which is silica, wherein the ferroferric oxide and the silica form a core-shell structure. The nanoparticle for absorbing a microwave provided by the invention can be used for effectively blocking electromagnetic interference.
Description
Technical field
The present invention relates to a kind of nanoparticle for absorbing microwave and synthetic method thereof, more particularly, the present invention relates to a kind of nanoparticle and synthetic method thereof of core-shell structure of the usefulness coated with silica Z 250 for absorbing microwave.
Background technology
Along with radio communication and high-frequency electronic equipment the developing rapidly of mega hertz scope, people pay close attention to electromagnetic interference problem more and more.In order to address this problem, multiple microwave absorbing material has obtained broad research.Therefore, the material that needs a kind of effectively block electromagnetic wave excitation.
Summary of the invention
In order to solve the problems of the prior art, the invention provides a kind of nanoparticle for absorbing microwave, described nanoparticle comprises: base material, described base material are Z 250; Shell, described shell are silicon-dioxide, and wherein, described Z 250 and described silicon-dioxide form nucleocapsid structure.
Preferably, described Z 250 is for being of a size of the nano particle of 7nm ~ 8nm, and the thickness of described silicon-dioxide is 11nm ~ 35nm.
In addition, the invention provides a kind of synthetic method of the nanoparticle for absorbing microwave, described synthetic method may further comprise the steps: the ferroferric oxide nano granules that (1) adopts hot solvent method preparation size is 7 ~ 8nm, have monodispersity; (2) adopt sol-gel method hydrolysis orthosilicic acid tetrem fat, at ferroferric oxide nano granules surface coated silica shell, thus the nano particle of the nucleocapsid structure of preparation coated with silica Z 250.
According to the present invention, step (1) comprising: ferric acetyl acetonade is dissolved in the polyvalent alcohol, and magnetic stirring, and carry out the high-purity argon gas protection; Solution is warming up to 100 ℃ ~ 130 ℃, is incubated 1 ~ 2 hour, then solution temperature is rapidly heated to the solution boiling, be incubated 2 ~ 6 hours; Reaction soln is cooled to room temperature, in reaction soln, adds ethyl acetate, and separate the Z 250 precipitation with kicker magnet; Behind dehydrated alcohol cleaning ferriferrous oxide nano-particle several, ferroferric oxide nano granules is added in the dehydrated alcohol, obtain the aaerosol solution of ferroferric oxide nano granules.
Preferably, the mass/volume of ferric acetyl acetonade and polyvalent alcohol is counted 0.035 ~ 0.06:1 than by g:mL; Described polyvalent alcohol is a kind of in triethylene glycol, the polyoxyethylene glycol.The volume ratio that adds ethyl acetate and reaction soln is 0.5 ~ 2:1.
According to the present invention, step (2) comprising: the ferroferric oxide nano granules suspension of preparation in the step (1) is added in the aqueous isopropanol mechanical stirring; Splash into ammoniacal liquor, regulating the pH value is 8 ~ 10; Add tetraethoxysilance, reacted 3 ~ 6 hours; Centrifugation and the particle of using washed with de-ionized water, drying to obtain.
According to the present invention, can regulate by the amount of regulating the tetraethoxy that adds the thickness of silica shell.
According to the effectively block electromagnetic interference of nanoparticle for absorbing microwave of the present invention.
Description of drawings
By reference accompanying drawing detailed description of the present invention, the features and advantages of the present invention will become and be more readily understood, in the accompanying drawings:
Fig. 1 is transmission electron microscope (TEM) photo that illustrates according to the ferroferric oxide nano granules of embodiment 1 preparation;
Fig. 2 is transmission electron microscope (TEM) photo that illustrates according to the ferroferric oxide nano granules of embodiment 2 preparations;
Fig. 3 is the graphic representation that is illustrated in the reflection loss of the ferroferric oxide nano granules of preparation among the embodiment 2;
Fig. 4 is transmission electron microscope (TEM) photo that is illustrated in the nanoparticle of the coated with silica Z 250 core-shell structure that drips different tetraethoxy preparations of measuring among the embodiment 3;
Fig. 5 is the reflection loss graphic representation that is illustrated in the coated with silica ferroferric oxide nano granules of measuring among the embodiment 3.
Embodiment
Ferrite is as the most conventional electromagnetic absorber, because it still has higher magnetic permeability under high frequency, and resistance is also larger, and hertzian wave enters and fast loss easily, so be widely used in radar and electromagnetic protection field.
Nano material is more much bigger than micron-sized powder to electromagnetic transmissivity and specific absorption.Nano material has fabulous absorption characteristic, have simultaneously broadband, compatible good, quality light and the characteristics such as thin thickness.Z 250 obtains extensive concern as a kind of important Ferrite Material in the microwave absorbing field.And SiO
2The basic role of shell component is that magnetoelectricity attribute and the magnetic core of itself mated mutually, produces specific magnetoelectricity phenomenon.In addition, SiO
2Shell also can be used for protection, stabilized magnetic core, and makes the composite particles surface have certain function.
The present invention adopts SiO
2Shell coated ferriferrous oxide particle, SiO
2Be good and economic general dielectric substance, by changing experiment condition, can control well SiO
2The thickness of shell is conducive to the adjusting of impedance matching, improves the absorbing property of matrix material.
Nanoparticle for absorbing microwave according to the present invention is the core-shell structure of coated with silica Z 250, and wherein, this nanoparticle is the composite particles of ball/hull shape shape.Specifically, the nanoparticle for absorbing microwave of the present invention comprises base material and shell, and wherein, base material is ferroferric oxide nano granules, and shell is silicon-dioxide.
Synthetic method according to the nanoparticle for absorbing microwave of the present invention may further comprise the steps: the ferroferric oxide nano granules that (1) adopts the hot solvent method to prepare mean sizes is 7 ~ 8nm, have monodispersity; (2) adopt sol-gel method hydrolysis orthosilicic acid tetrem fat, at ferroferric oxide nano granules surface coated silica shell, thus the nano particle of the nucleocapsid structure of preparation coated with silica Z 250.
In the superincumbent step (1), adopt and come in the following method to synthesize ferriferrous oxide nano-particle: an amount of ferric acetyl acetonade is dissolved in the polyvalent alcohol, magnetic stirring, and carry out the high-purity argon gas protection; Solution temperature is risen to 100 ℃ ~ 130 ℃, be incubated 1 ~ 2 hour, then solution temperature is rapidly heated to the solution boiling, be incubated 2 ~ 6 hours; Reaction soln is cooled to room temperature, adds a certain amount of ethyl acetate in reaction soln, wherein, the volume ratio of ethyl acetate and former reaction soln is 0.5 ~ 2:1, and separates the Z 250 precipitation with kicker magnet; Behind dehydrated alcohol cleaning ferriferrous oxide nano-particle several, ferroferric oxide nano granules is added in the dehydrated alcohol, obtain the aaerosol solution of ferroferric oxide nano granules.
Wherein, the mass/volume of ferric acetyl acetonade and polyvalent alcohol is than counting 0.035 ~ 0.06:1 by g:mL.
Described polyvalent alcohol can be in triethylene glycol, the polyoxyethylene glycol a kind of.
When polyvalent alcohol is triethylene glycol, solution temperature is being rapidly heated to the step of solution boiling, be rapidly heated solution temperature to 280 ℃ and be incubated 2 ~ 6 hours.When polyvalent alcohol is polyoxyethylene glycol, solution is being rapidly heated to the step of solution boiling, be rapidly heated solution temperature to 300 ℃ and be incubated 2 ~ 6 hours.
In the superincumbent step (2), the step that forms nucleocapsid structure with the coated with silica Z 250 is: be in the ferroferric oxide nano granules suspension adding aqueous isopropanol of 7 ~ 8nm with the particle diameter for preparing in the step (1), and mechanical stirring; Splash into ammoniacal liquor, regulating the pH value is 8 ~ 10; Add an amount of tetraethoxysilance again, reacted 3 ~ 6 hours, centrifugation is also used washed with de-ionized water, and the particle that obtains is dry in vacuum drying oven.
Alternatively, the ammoniacal liquor that adopts in the above can be the ammoniacal liquor of 25wt% for concentration.
For the ferroferric oxide nano granules of 0.2g, be respectively the tetraethoxy of 200uL, 600uL, 1200uL by adding, obtain the SiO of a series of different thickness
2The sample of shell.The thickness of the silica shell that obtains in the present invention, is 11nm ~ 35nm.
The below will describe according to a particular embodiment of the invention.
The preparation of embodiment 1 ferroferric oxide nano granules
Be that 0.035:1 gets ferric acetyl acetonade and polyoxyethylene glycol according to mass/volume than g:mL, the ferric acetyl acetonade of 1.75g is dissolved in the polyoxyethylene glycol of 50mL, solution is poured in the there-necked flask, magnetic stirring, and carry out the high-purity argon gas protection.Solution temperature is risen to 120 ℃ first, be incubated 1 hour, solution temperature is rapidly heated to 300 ℃ again, be incubated 2 hours.Reaction soln is cooled to room temperature, adds the 50mL ethyl acetate, and separate the Z 250 precipitation with kicker magnet.With dehydrated alcohol clean ferriferrous oxide nano-particle for several times after, with ferroferric oxide nano granules 50 ℃ of dryings 24 hours in vacuum drying oven.
The Fe of Fig. 1 for preparing in polyglycol solution according to embodiment 1
3O
4The TEM figure of nano particle.Nano particle is overlapped as seen from Figure 1, and it is serious to reunite, and is dispersed not so good, but granule-morphology is sphere, all has single crystal structure, and the size of particle is about 7 ~ 9nm.Also indicated the lattice plane spacing of a plurality of particles among Fig. 1, be about 2.53A, near face-centered cubic Fe
3O
4(311) interplanar distance.
Preparation and the microwave absorbing research of embodiment 2 even ferroferric oxide nano granules
Be that 0.035:1 gets ferric acetyl acetonade and triethylene glycol according to mass/volume than by g:mL, the ferric acetyl acetonade of 1.75g is dissolved in the triethylene glycol of 50mL, solution is poured in the there-necked flask, magnetic stirring, and carry out the high-purity argon gas protection.Solution temperature is risen to 120 ℃ first, be incubated 1 hour, again the temperature temperature is rapidly heated to 280 ℃, be incubated 2 hours.The reaction soln temperature is down to room temperature, adds the 50mL ethyl acetate, and separate the Z 250 precipitation with kicker magnet.With dehydrated alcohol clean ferriferrous oxide nano-particle for several times after, with ferroferric oxide nano granules 50 ℃ of dryings 24 hours in vacuum drying oven.
Fig. 2 shows the transmission electron microscope photo according to the Z 250 of embodiment 2 preparations.As seen from Figure 2, the gained ferriferrous oxide particles is globosity, and the size of particle is about 7 ~ 8nm; Compare with the ferriferrous oxide particles of preparation in the embodiment 1, have better monodispersity, distribution of sizes is more even; Prepared particle is single crystal structure.
The finely dispersed ferroferric oxide nano granules that obtains is mixed for 1:4 in mass ratio with paraffin, make the annulus of internal diameter 3mm external diameter 7mm, utilize vector network analyzer coaxial line method to carry out electromagnetic parameter testing, the test frequency scope is 1-18GHz, and utilizes the reflectivity of electromagnetic transmission lineation opinion calculation sample when different thickness.Fig. 3 is the reflection loss figure of the ferroferric oxide nano granules that obtains.As can be seen from Figure 3, the reflection loss of sample increases with the increase of annulus thickness, and the trend that moves with the oriented low frequency of the increase of thickness of reflection loss peak value.
Preparation and the microwave absorbing research of embodiment 3 coated with silica Z 250 nucleocapsid particles
The ferroferric oxide nano granules that obtains among the embodiment 2 is added in the 20mL dehydrated alcohol, make the suspension of Z 250.Get 2.25mL suspension and add in the 150mL aqueous isopropanol mechanical stirring; Splash into first the ammoniacal liquor that the 4.5mL massfraction is 25wt%, regulating the pH value is 8.5; Add an amount of tetraethoxysilance (amount that adds tetraethoxysilance is respectively: 200uL, 600uL, 1200uL) again, reacted 3 hours, centrifugation is also used washed with de-ionized water, and the particle that obtains is dry in vacuum drying oven.
(Fig. 4) can find out by the transmission electron microscope photo, and when the add-on of tetraethoxysilance was 1200uL, the thickness of coated with silica layer coated evenly about 30nm, and nucleocapsid particles is chain.When the amount that adds tetraethoxysilance was 200uL and 600uL, the thickness that obtains the coated with silica layer was about respectively 11nm, 20nm.
Mix for 1:4 with the Quality of Paraffin Waxes ratio obtaining the nucleocapsid particles of coated with silica layer about 30nm, make the annulus of internal diameter 3mm external diameter 7mm, utilize vector network analyzer coaxial line method to carry out electromagnetic parameter testing.The test frequency scope is 1-18GHz, and utilizes the reflectivity of electromagnetic transmission lineation opinion calculation sample when different thickness.Fig. 5 is the reflection loss figure that obtains, and as can be seen from Figure 5, along with the increase of annulus thickness, the variation tendency of reflection loss curve is basic identical with the plots changes of coatedparticles not.Total reflection loss value diminishes after coating, but the reflection loss peak value all moves to high frequency direction.The present invention adopts classics
Method hydrolysis orthosilicic acid tetrem fat coats the silica shell of preparation even thickness to the water-soluble ferroferric oxide nano particle.In addition, can coat by the concentration adjustment that changes presoma the thickness of shell.
The present invention utilizes the ferric acetyl acetonade decomposes, and utilizes polyvalent alcohol as reaction carriers and dispersion agent by solvent-thermal method, can obtain the ferroferric oxide nano granules that monodispersity is good, be of a size of 7 ~ 8nm under the temperature of solvent thermal and shielding gas.Compare with the synthetic of ferroferric oxide nano granules of the prior art, have the following advantages: 1) the present invention does not need to add other stablizer and dispersion agent, and polyvalent alcohol itself is reaction solvent, be again the dispersion agent of particle, so aftertreatment technology is simple; 2) required chemical reagent kind is few, and does not all have toxicity, operational safety; 3) the ferroferric oxide nano granules narrow diameter distribution of the present invention's preparation has monodispersity, good water solubility, and experimental repeatability is good.
In the preparation process step (2), adopt tetraethoxysilance to be decomposed into Z 250 coated silica layer, method is simple and easy to control, the cycle is short, need not heating and coating is even, and thickness is controlled.
Claims (10)
1. nanoparticle that is used for absorbing microwave, described nanoparticle comprises:
Base material, described base material are Z 250;
Shell, described shell are silicon-dioxide,
Wherein, described Z 250 and described silicon-dioxide form nucleocapsid structure.
2. nanoparticle according to claim 1, wherein, described Z 250 is for being of a size of the nano particle of 7nm ~ 8nm.
3. nanoparticle according to claim 1, wherein, the thickness of described silicon-dioxide is 11nm ~ 35nm.
4. synthetic method that is used for the nanoparticle of absorbing microwave, described synthetic method may further comprise the steps:
(1) ferroferric oxide nano granules that to adopt hot solvent method preparation size be 7 ~ 8nm, have monodispersity;
(2) adopt sol-gel method hydrolysis orthosilicic acid tetrem fat, at ferroferric oxide nano granules surface coated silica shell, thus the nano particle of the nucleocapsid structure of preparation coated with silica Z 250.
5. synthetic method according to claim 4, wherein, step (1) comprising:
Ferric acetyl acetonade is dissolved in the polyvalent alcohol, magnetic stirring, and carry out the high-purity argon gas protection;
Solution is warming up to 100 ℃ ~ 130 ℃, is incubated 1 ~ 2 hour, then solution temperature is rapidly heated to the solution boiling, be incubated 2 ~ 6 hours;
Reaction soln is cooled to room temperature, in reaction soln, adds ethyl acetate, and separate the Z 250 precipitation with kicker magnet;
Behind dehydrated alcohol cleaning ferriferrous oxide nano-particle several, ferroferric oxide nano granules is added in the dehydrated alcohol, obtain the aaerosol solution of ferroferric oxide nano granules.
6. synthetic method according to claim 5, wherein, the mass/volume of ferric acetyl acetonade and polyvalent alcohol is than counting 0.035 ~ 0.06:1 by g:mL.
7. synthetic method according to claim 5, wherein, described polyvalent alcohol is a kind of in triethylene glycol, the polyoxyethylene glycol.
8. synthetic method according to claim 5, wherein, the volume ratio that adds ethyl acetate and reaction soln is 0.5 ~ 2:1.
9. synthetic method according to claim 4, wherein, step (2) comprising:
The ferroferric oxide nano granules suspension of preparation in the step (1) is added in the aqueous isopropanol mechanical stirring;
Splash into ammoniacal liquor, regulating the pH value is 8 ~ 10;
Add tetraethoxysilance, reacted 3 ~ 6 hours;
Centrifugation and the particle of using washed with de-ionized water, drying to obtain.
10. synthetic method according to claim 9 wherein, is regulated the thickness of silica shell by the amount of regulating the tetraethoxy that adds.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528839A (en) * | 2015-01-15 | 2015-04-22 | 安徽大学 | Fe3O4 nanoparticle electromagnetic wave absorbent and preparation method thereof |
| CN104628422A (en) * | 2015-01-27 | 2015-05-20 | 济南大学 | Method for enabling cement or concrete to have wave absorbing performance and dense surface by using silicon dioxide (SiO2) coated magnetic nanoparticles |
| CN107776000A (en) * | 2016-08-25 | 2018-03-09 | 叶中豹 | One kind is used for the new ghost particulate composite Distribution Layer of civil air defense constructions and installations |
| CN108419426A (en) * | 2018-03-05 | 2018-08-17 | 沈阳航空航天大学 | Coated with silica magnetic graphene tiny balloon and its magnanimity preparation method |
| CN110724492A (en) * | 2019-09-29 | 2020-01-24 | 安徽理工大学 | Ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
| CN114106670A (en) * | 2021-12-23 | 2022-03-01 | 安徽神剑新材料股份有限公司 | Electromagnetic shielding powder coating and preparation method thereof |
| CN115820181A (en) * | 2022-12-07 | 2023-03-21 | 东莞市新懿电子材料技术有限公司 | Underfill adhesive based on composite nano filler and preparation method and application thereof |
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| CN1594450A (en) * | 2004-06-30 | 2005-03-16 | 南京大学 | Core/shell structure containing Fe/SiO2 composite nano particles with high stability and method for making same |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594450A (en) * | 2004-06-30 | 2005-03-16 | 南京大学 | Core/shell structure containing Fe/SiO2 composite nano particles with high stability and method for making same |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528839A (en) * | 2015-01-15 | 2015-04-22 | 安徽大学 | Fe3O4 nanoparticle electromagnetic wave absorbent and preparation method thereof |
| CN104528839B (en) * | 2015-01-15 | 2016-06-15 | 安徽大学 | A kind of Fe3O4Nanoparticle radio-radar absorber and preparation method thereof |
| CN104628422A (en) * | 2015-01-27 | 2015-05-20 | 济南大学 | Method for enabling cement or concrete to have wave absorbing performance and dense surface by using silicon dioxide (SiO2) coated magnetic nanoparticles |
| CN107776000A (en) * | 2016-08-25 | 2018-03-09 | 叶中豹 | One kind is used for the new ghost particulate composite Distribution Layer of civil air defense constructions and installations |
| CN108419426A (en) * | 2018-03-05 | 2018-08-17 | 沈阳航空航天大学 | Coated with silica magnetic graphene tiny balloon and its magnanimity preparation method |
| CN110724492A (en) * | 2019-09-29 | 2020-01-24 | 安徽理工大学 | Ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof |
| CN114106670A (en) * | 2021-12-23 | 2022-03-01 | 安徽神剑新材料股份有限公司 | Electromagnetic shielding powder coating and preparation method thereof |
| CN114106670B (en) * | 2021-12-23 | 2022-08-05 | 安徽神剑新材料股份有限公司 | Electromagnetic shielding powder coating and preparation method thereof |
| CN115820181A (en) * | 2022-12-07 | 2023-03-21 | 东莞市新懿电子材料技术有限公司 | Underfill adhesive based on composite nano filler and preparation method and application thereof |
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