CN105565394A - Preparation method of graphene hollow microspheres loaded with magnetic nanoparticles - Google Patents
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- CN105565394A CN105565394A CN201510925343.3A CN201510925343A CN105565394A CN 105565394 A CN105565394 A CN 105565394A CN 201510925343 A CN201510925343 A CN 201510925343A CN 105565394 A CN105565394 A CN 105565394A
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- C01G49/00—Compounds of iron
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- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention discloses a preparation method of graphene hollow microspheres loaded with magnetic nanoparticles. The method comprises the following steps: preparing a uniform oxidized graphene hollow microsphere precursor loaded with a metal salt by taking oxidized graphene, polyvinyl alcohol and the metal salt as raw materials through a water-in-oil inverse emulsion method; performing roasting reduction under a protective atmosphere to obtain the graphene hollow microspheres loaded with the magnetic nanoparticles. By adopting the method, the problems that the binding force between the graphene and the magnetic particles is insufficient, the magnetic particles cannot be uniformly loaded on graphene, the magnetic particles are agglomerated and the like in the prior art are solved; the prepared hollow microspheres have the characteristics of large specific surface area and small density, and the inner and outer surfaces of the microspheres and the insides of sphere walls are loaded with the magnetic nanoparticles. The magnetic performance and electrical performance of a material can be adjusted by adjusting the proportion of the graphene to the metal salt. A graphene hollow microsphere material loaded with the magnetic nanoparticles prepared by the method has excellent electromagnetic performance, and can be applied to electromagnetic wave absorbing materials.
Description
Technical field
The present invention relates to a kind of preparation method of graphene hollow microspheres of carried magnetic nano particle.
Background technology
Modern war, grasp the active that mastery of the air just grasps war, and grasp mastery of the air weapon be exactly aircraft, but in war, strategic objective fixing on ground, aeroamphibious weapon system-of-systems and personnel at all levels's moment are all in aerial dynamic of the monitoring of various radar-probing system, so the stealthy technique of aircraft improve modern armament penetration ability in play an important role, therefore absorbing material as the key factor of stealthy technique by countries in the world focus development.
Along with the development of modern science and technology, the impact of electromagenetic wave radiation on environment increases day by day.On airport, airplane flight is overdue because Electromagnetic Interference cannot be taken off; In hospital, mobile telephone often can disturb the normal work of various electronic instrument for diagnosing and curing diseases device.The electromagnetic interference that electromagnetic radiation causes not only can affect the normal operation of various electronics, and also has very large harm to the health that the person is very psychological.Particularly after traditional metal materials is substituted by plastics, electromangnetic spectrum just seems more important, and to study electromangnetic spectrum most critical be research to absorbing material and coating.Use absorbing material as the coating of electromangnetic spectrum, not only with low cost, simple process and electromagnetic pollution can be suppressed efficiently, therefore study the important topic that the electromagnetic shielding material of excellent performance and absorbing material become scientific research person's research
At present, following two aspects are mainly concentrated on to the research of absorbing material both at home and abroad: develop the new nano-powder with absorbing property; Existing nano wave-absorbing material is adulterated or compound, makes its absorbing property improve and improve.Aforesaid method exists that efficiency is low, frequency is large and the shortcoming such as density is large simultaneously, and these shortcomings make the application of absorbing material be subject to certain restrictions, and therefore how making high performance absorbing material becomes developing direction.
At present the research of absorbing material is required that it should have: thin, light, wide, strong.I.e. light, the bandwidth of thin, the quality of thickness, feature that suction ripple is strong.
Graphene is the thinnest known a kind of material, but very firmly hard, and it is also stronger than diamond, the best iron and steel taller hundred times of its strength ratio it be also the conductive material that known at present performance is outstanding, its electronic movement velocity is 1/300 of the light velocity, electronic movement velocity in general conductor, moreover, the good (5000Wm of Graphene thermal conductivity
-1k
-1), the large (2630m of specific surface area
2g
-1), its Young's modulus (1100GPa) and breaking tenacity (125GPa) also can compare favourably with carbon nanotube.Graphene mainly plays dielectric loss to hertzian wave, but the electroconductibility of Graphene is very good destroys impedance matching on the contrary, and its wave absorbtion is declined.
Magnetic Nano material is the focus of modern absorbing material research, and magnetic nano-particle plays the effect of magnetic loss to hertzian wave, and mainly shows excellent wave absorbtion at high frequency treatment.Owing to there is the shortcoming of easily reuniting, dispersing nanometer magnetic particle is a difficult point.
In order to make material electromagnetic wave absorption greatly, investigators are prepared into composite wave absorption material the material of dielectric loss and magnetic loss, and the research of graphene composite material based on this is also a study hotspot now.
Summary of the invention
The invention provides a kind of preparation method of graphene hollow microspheres of carried magnetic nano particle, the method for raw material, has the graphene oxide tiny balloon presoma of metal-salt with the metal-salt of graphene oxide, polyvinyl alcohol and iron, cobalt, nickel for a kind of uniform load by water-in-oil inverse emulsion legal system; And under protective atmosphere roasting reduction, obtain the graphene hollow microspheres of carried magnetic nano particle.This method solve Graphene and magnetic particle bonding force in prior art not enough, magnetic particle can not uniform loading on Graphene, magnetic particle such as easily to be reunited at the problem.The graphene hollow microspheres of the carried magnetic nano particle of preparation has the low-density feature of high-ratio surface sum, by adjusting magnetic property and the dielectric properties of the add-on regulable control microballoon of metal-salt and graphene oxide.
In order to achieve the above object, technical solution of the present invention is:
A preparation method for the graphene hollow microspheres of carried magnetic nano particle, comprises the following steps:
(1) graphene oxide, deionized water, liquid alcohols, polyvinyl alcohol and metal-salt are configured to reaction solution by a certain percentage;
The ratio of described reaction solution is graphene oxide: deionized water: liquid alcohols: polyvinyl alcohol: metal-salt=30-80mg:6-10ml:12-22ml:100-300mg:200-500mg; Described oil comprises one in methyl-silicone oil, dimethyl silicone oil, soybean oil, peanut oil, sweet oil, Semen Benincasae oil, tea-seed oil, rapeseed oil and combination thereof; Described metal-salt comprises one in ferric acetyl acetonade, acetylacetonate nickel, acetylacetone cobalt, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, iron nitrate, nickelous nitrate, ironic acetate, cobaltous acetate, nickelous acetate, iron(ic) chloride, nickelous chloride, cobalt chloride and combination thereof; Described liquid alcohols comprises ethanol, methyl alcohol or the two mixture.
(2) add in reaction vessel by 150-250ml oil, heating in water bath is to 60-75 DEG C; Under the stirring velocity of 5000r/min-6000r/min, the reaction solution that step (1) configures slowly is added dropwise in oil and stirs 5-10 minute, form water in oil reaction system; Stirring velocity is down to 500-1000r/min and stirs 3-5 hour; By warming-in-water to 90-100 DEG C, continue to stir after 3-5 hour under the stirring velocity of 500-1000r/min; Finally by reacting liquid filtering, with deionized water wash, dry under 60-80 DEG C of vacuum condition, obtain the graphene oxide tiny balloon presoma that load has metal-salt.
(3) graphene oxide tiny balloon presoma step (2) obtained, heat up calcining 0.5-4 hour in protective atmosphere, cool to graphene oxide tiny balloon presoma with the furnace room temperature, namely obtain the graphene hollow microspheres of carried magnetic nano particle;
Described protection gas bag draws together nitrogen, argon gas, neon, the one of helium and combination thereof, and shielding gas flow amount is 40-100ml/min; Described temperature rise rate is 1-10 DEG C/min; Described calcining temperature is 300-800 DEG C.
The be magnetic graphene hollow microspheres material of nanoparticle of load prepared by the present invention has excellent electromagnetic performance, may be used for electromagnetic wave absorbent material.
Beneficial effect of the present invention is: 1. the Graphene microballoon of preparation is hollow, sphere diameter is 5-10 micron, can increase the specific surface area of material, reduces the density of material, have the advantages that specific surface area is high and density is little, the surfaces externally and internally of microballoon and the equal load of ball pars intramuralis are magnetic nanoparticle; 2. magnetic nano-particle load is between graphene sheet layer, not only solves the problem that magnetic nano-particle is reunited, also solves the agglomeration traits of Graphene itself simultaneously; 3. by regulating the proportioning of Graphene and magnetic nano-particle, the electromagnetic performance class of material being regulated, greatly having widened material as effective frequency range when wave-absorbing and camouflage and electromagnetic shielding material.The be magnetic graphene hollow microspheres material of nanoparticle of load prepared by the present invention has excellent electromagnetic performance, may be used for electromagnetic wave absorbent material.
Accompanying drawing explanation
Fig. 1 is load ferriferrous oxide nano-particle Graphene microballoon surface sweeping Electronic Speculum figure prepared by embodiment 2.
Fig. 2 is that embodiment 2 prepares load ferriferrous oxide nano-particle Graphene microballoon minority because the scanning electron microscope (SEM) photograph that breaks of high temperature.
Fig. 3 is the microwave electromagnetic reflecting properties test result figure that embodiment 1-4 prepares load ferriferrous oxide nano-particle Graphene microballoon.
Fig. 4 is the microwave electromagnetic reflecting properties test result figure that embodiment 2 prepares the simulation different thickness of load ferriferrous oxide nano-particle Graphene microballoon.
Embodiment
Embodiment 1:
Step 1: add 40mg graphene oxide in the beaker of 50ml, then adds 7ml deionized water, supersound process 30 minutes; Take 100mg polyvinyl alcohol to add in the mixed solution of graphene oxide and water, be stirred to polyvinyl alcohol and all dissolve, be designated as A liquid.Get one, 50ml beaker, measure 12ml ethanol and add in beaker, take 200mg ferric acetyl acetonade and add in beaker, be stirred to ferric acetyl acetonade and all dissolve, be designated as B liquid; By A liquid and the mixing of B liquid, and stir, obtain reaction solution.
Step 2: get 500ml there-necked flask one, add 200ml sweet oil, flask is put into 65 DEG C of water-baths and is heated, and uses stirrer to stir, and stirring velocity is 5000r/min.Reaction solution step 2 prepared slowly is added dropwise in flask, after dripping under the speed of 5000r/min Keep agitation 5min, then stirring velocity is down to 500r/min, Keep agitation 3 hours; Water-bath is risen to 90 DEG C, and under 500r/min rotating speed, continue stirring 3 hours, stop afterwards stirring; Filtering reacting liquid, with washed with de-ionized water filter cake twice, the vacuum-drying at 70 DEG C of last filter cake, obtains load ferric acetyl acetonade graphene oxide microballoon presoma.
Step 3: the load ferric acetyl acetonade graphene oxide microballoon that step 2 obtains is put into crucible; crucible is put into the silica tube of tube furnace; in silica tube, pass into argon gas, airshed is 50ml/min, ventilates after 20 minutes; it is 5 DEG C/min that stove starts temperature rise rate; arranging calcining temperature is 400 DEG C, and calcination time is 2 hours, cools to room temperature with the furnace afterwards; close shielding gas, obtain the graphene hollow microspheres of carried magnetic nano particle.
Embodiment 2:
Step 1: add 50mg graphene oxide in the beaker of 50ml, then adds 7ml deionized water, supersound process 30 minutes; Take 200mg polyvinyl alcohol to add in the mixed solution of graphene oxide and water, be stirred to polyvinyl alcohol and all dissolve, be designated as A liquid.Get one, 50ml beaker, measure 15ml ethanol and add in beaker, take 300mg ferric acetyl acetonade and add in beaker, be stirred to ferric acetyl acetonade and all dissolve, be designated as B liquid; By A liquid and the mixing of B liquid, and stir, obtain reaction solution.
Step 2: get 500ml there-necked flask one, add 200ml sweet oil, flask is put into 70 DEG C of water-baths and is heated, and uses stirrer to stir, and stirring velocity is 6000r/min.Reaction solution step 2 prepared slowly is added dropwise in flask, after dripping under the speed of 6000r/min Keep agitation 10min, then stirring velocity is down to 800r/min, Keep agitation 4 hours; Water-bath is risen to 95 DEG C, and under 800r/min rotating speed, continue stirring 4 hours, stop afterwards stirring; Filtering reacting liquid, with washed with de-ionized water filter cake twice, the vacuum-drying at 75 DEG C of last filter cake, obtains load ferric acetyl acetonade graphene oxide microballoon presoma.
Step 3: the load ferric acetyl acetonade graphene oxide microballoon that step 2 obtains is put into crucible; crucible is put into the silica tube of tube furnace; in silica tube, pass into argon gas, airshed is 60ml/min, ventilates after 20 minutes; it is 7 DEG C/min that stove starts temperature rise rate; arranging calcining temperature is 500 DEG C, and calcination time is 2 hours, cools to room temperature with the furnace afterwards; close shielding gas, obtain the graphene hollow microspheres of carried magnetic nano particle.
Embodiment 3:
Step 1: add 70mg graphene oxide in the beaker of 50ml, then adds 10ml deionized water, supersound process 30 minutes; Take 300mg polyvinyl alcohol to add in the mixed solution of graphene oxide and water, be stirred to polyvinyl alcohol and all dissolve, be designated as A liquid.Get one, 50ml beaker, measure 20ml ethanol and add in beaker, take 400mg ferric acetyl acetonade and add in beaker, be stirred to ferric acetyl acetonade and all dissolve, be designated as B liquid; By A liquid and the mixing of B liquid, and stir, obtain reaction solution.
Step 2: get 500ml there-necked flask one, add 200ml sweet oil, flask is put into 75 DEG C of water-baths and is heated, and uses stirrer to stir, and stirring velocity is 6000r/min.Reaction solution step 2 prepared slowly is added dropwise in flask, after dripping under the speed of 6000r/min Keep agitation 10min, then stirring velocity is down to 1000r/min, Keep agitation 5 hours; Water-bath is risen to 100 DEG C, and under 1000r/min rotating speed, continue stirring 5 hours, stop afterwards stirring; Filtering reacting liquid, with washed with de-ionized water filter cake twice, the vacuum-drying at 80 DEG C of last filter cake, obtains load ferric acetyl acetonade graphene oxide microballoon presoma.
Step 3: the load ferric acetyl acetonade graphene oxide microballoon that step 2 obtains is put into crucible; crucible is put into the silica tube of tube furnace; in silica tube, pass into argon gas, airshed is 90ml/min, ventilates after 20 minutes; it is 10 DEG C/min that stove starts temperature rise rate; arranging calcining temperature is 600 DEG C, and calcination time is 4 hours, cools to room temperature with the furnace afterwards; close shielding gas, obtain the graphene hollow microspheres of carried magnetic nano particle.
Embodiment 4:
Step 1: add 80mg graphene oxide in the beaker of 50ml, then adds 10ml deionized water, supersound process 30 minutes; Take 300mg polyvinyl alcohol to add in the mixed solution of graphene oxide and water, be stirred to polyvinyl alcohol and all dissolve, be designated as A liquid.Get one, 50ml beaker, measure 20ml ethanol and add in beaker, take 400mg ferric acetyl acetonade and add in beaker, be stirred to ferric acetyl acetonade and all dissolve, be designated as B liquid; By A liquid and the mixing of B liquid, and stir, obtain reaction solution.
Step 2: get 500ml there-necked flask one, add 200ml sweet oil, flask is put into 75 DEG C of water-baths and is heated, and uses stirrer to stir, and stirring velocity is 5000r/min.Reaction solution step 2 prepared slowly is added dropwise in flask, after dripping under the speed of 5000r/min Keep agitation 5min, then stirring velocity is down to 500r/min, Keep agitation 3 hours; Water-bath is risen to 95 DEG C, and under 500r/min rotating speed, continue stirring 3 hours, stop afterwards stirring; Filtering reacting liquid, with washed with de-ionized water filter cake twice, the vacuum-drying at 80 DEG C of last filter cake, obtains load ferric acetyl acetonade graphene oxide microballoon presoma.
Step 3: the load ferric acetyl acetonade graphene oxide microballoon that step 2 obtains is put into crucible; crucible is put into the silica tube of tube furnace; in silica tube, pass into argon gas, airshed is 60ml/min, ventilates after 20 minutes; it is 5 DEG C/min that stove starts temperature rise rate; arranging calcining temperature is 800 DEG C, and calcination time is 4 hours, cools to room temperature with the furnace afterwards; close shielding gas, obtain the graphene hollow microspheres of carried magnetic nano particle.
Claims (8)
1. a preparation method for the graphene hollow microspheres of carried magnetic nano particle, is characterized in that, comprises the following steps:
(1) 30-80mg graphene oxide, 6-10ml deionized water, 12-22ml liquid alcohols, 100-300mg polyvinyl alcohol and 200-500mg metal-salt are configured to reaction solution;
(2) add in reaction vessel by 150-250ml oil, heating in water bath is to 60-75 DEG C;
By in step (1) reaction solution instillation oil under the stirring velocity of 5000r/min-6000r/min, stir 5-10 minute;
Stirring velocity is down to 500-1000r/min and stirs 3-5 hour;
By warming-in-water to 90-100 DEG C, then stir 3-5 hour;
Finally by reacting liquid filtering, obtain with the drying of deionized water wash final vacuum the graphene oxide tiny balloon presoma that load has metal-salt;
(3) graphene oxide tiny balloon presoma step (2) obtained, is warming up to 300-800 DEG C by 1-10 DEG C/min in protective atmosphere, calcining 0.5-4 hour; Cool to graphene oxide tiny balloon presoma with the furnace room temperature, obtain the graphene hollow microspheres of carried magnetic nano particle.
2. preparation method as claimed in claim 1, it is characterized in that, described metal-salt comprises ferric acetyl acetonade, acetylacetonate nickel, acetylacetone cobalt, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, iron nitrate, nickelous nitrate, ironic acetate, cobaltous acetate, nickelous acetate, iron(ic) chloride, nickelous chloride, the one of cobalt chloride and combination thereof.
3. preparation method as claimed in claim 1 or 2, is characterized in that, described oil comprises one in methyl-silicone oil, dimethyl silicone oil, soybean oil, peanut oil, sweet oil, Semen Benincasae oil, tea-seed oil, rapeseed oil and combination thereof.
4. preparation method as claimed in claim 1 or 2, it is characterized in that, described liquid alcohols comprises ethanol, methyl alcohol or the two mixture.
5. preparation method as claimed in claim 3, it is characterized in that, described liquid alcohols comprises ethanol, methyl alcohol or the two mixture.
6. the preparation method as described in claim 1 or 2 or 5, is characterized in that, described protection gas bag draws together nitrogen, argon gas, neon, the one of helium and combination thereof, and shielding gas flow amount is 40-100ml/min.
7. preparation method as claimed in claim 3, is characterized in that, described protection gas bag draws together nitrogen, argon gas, neon, the one of helium and combination thereof, and shielding gas flow amount is 40-100ml/min.
8. preparation method as claimed in claim 4, is characterized in that, described protection gas bag draws together nitrogen, argon gas, neon, the one of helium and combination thereof, and shielding gas flow amount is 40-100ml/min.
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| CN108190866A (en) * | 2018-03-02 | 2018-06-22 | 山东大学 | A kind of method that water-in-oil emulsion method simply controls synthesis sea urchin shape graphene ball |
| 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 |
| CN108439376A (en) * | 2018-03-21 | 2018-08-24 | 大连理工大学 | A kind of preparation method of the graphene aerogel composite material of carried magnetic nano particle |
| CN110564365A (en) * | 2019-09-03 | 2019-12-13 | 大连理工大学 | Preparation method of graphene foam composite material loaded with magnetic hollow nanospheres |
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| CN117487474A (en) * | 2023-11-07 | 2024-02-02 | 江苏斯瑞达材料技术股份有限公司 | Pressure-sensitive adhesive tape with electromagnetic shielding function and preparation method thereof |
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| CN107418511A (en) * | 2017-05-25 | 2017-12-01 | 大连理工大学 | The preparation method of FeCo/ redox graphene composite wave-suction materials |
| CN107418511B (en) * | 2017-05-25 | 2019-11-08 | 大连理工大学 | The preparation method of FeCo/ redox graphene composite wave-suction material |
| CN108190866A (en) * | 2018-03-02 | 2018-06-22 | 山东大学 | A kind of method that water-in-oil emulsion method simply controls synthesis sea urchin shape graphene ball |
| CN108190866B (en) * | 2018-03-02 | 2021-07-23 | 山东大学 | Method for simply controlling synthesis of echinoid graphene spheres by water-in-oil emulsion method |
| 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 |
| CN108419426B (en) * | 2018-03-05 | 2019-11-22 | 沈阳航空航天大学 | Coated with silica magnetic graphene tiny balloon and its magnanimity preparation method |
| CN108439376A (en) * | 2018-03-21 | 2018-08-24 | 大连理工大学 | A kind of preparation method of the graphene aerogel composite material of carried magnetic nano particle |
| CN110564365A (en) * | 2019-09-03 | 2019-12-13 | 大连理工大学 | Preparation method of graphene foam composite material loaded with magnetic hollow nanospheres |
| CN110564365B (en) * | 2019-09-03 | 2021-06-04 | 大连理工大学 | Preparation method of graphene foam composite material loaded with magnetic hollow nanospheres |
| CN115215334A (en) * | 2022-07-19 | 2022-10-21 | 重庆交通大学 | Preparation method of graphene oxide aerogel hollow microspheres |
| CN115215334B (en) * | 2022-07-19 | 2023-05-05 | 重庆交通大学 | Preparation method of graphene oxide aerogel hollow microspheres |
| CN117487474A (en) * | 2023-11-07 | 2024-02-02 | 江苏斯瑞达材料技术股份有限公司 | Pressure-sensitive adhesive tape with electromagnetic shielding function and preparation method thereof |
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