CN105565394B - A kind of preparation method of the graphene hollow microspheres of carried magnetic nano particle - Google Patents
A kind of preparation method of the graphene hollow microspheres of carried magnetic nano particle Download PDFInfo
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Abstract
A kind of preparation method of the graphene hollow microspheres of carried magnetic nano particle, this method prepares the uniform graphene oxide tiny balloon presoma for being loaded with metal salt using graphene oxide, polyvinyl alcohol and metal salt as raw material with water-in-oil inverse emulsion method；The roasting reduction under protective atmosphere, obtains the graphene hollow microspheres of carried magnetic nano particle.It this method solve graphene in the prior art and magnetic particle adhesion be not enough, magnetic particle is unable to uniform load on graphene, the problems such as magnetic particle is reunited；The characteristics of prepared tiny balloon has specific surface area height and small density, the surfaces externally and internally and ball pars intramuralis of microballoon are loaded with magnetic nano-particle.By adjusting the proportioning of graphene and metal salt, the magnetic property and electrical property of material can be adjusted.The graphene hollow microspheres material that prepared by the present invention be loaded with magnetic nano-particle has excellent electromagnetic performance, can be used for electromagnetic wave absorbent material.
Description
Technical field
The present invention relates to a kind of preparation method of the graphene hollow microspheres of carried magnetic nano particle.
Background technology
Modern war, grasps the active that control of the air just grasps war, and the weapon for grasping control of the air is exactly aircraft, still
In war, fixed strategic objective, aeroamphibious weapon system-of-systems and personnel at all levels are at various constantly on ground
The aerial dynamic of monitoring of radar-probing system, so the stealth technology of aircraft is sent out in terms of the penetration ability of modern armament is improved
Wave important effect, thus absorbing material as the key factor of stealth technology by countries in the world focus development.
With the development of modern science and technology, influence of the electromagenetic wave radiation to environment increasingly increases.On airport, airplane flight
Because Electromagnetic Interference can not take off and it is overdue；In hospital, mobile phone can often disturb the normal work of various electronic instrument for diagnosing and curing diseases devices.
The electromagnetic interference that electromagnetic radiation is caused can not only influence the normal operation of various electronics, and to the human body very heart
The health of reason also has very big harm.Particularly after traditional metal materials are substituted by plastic products, electromangnetic spectrum just shows
Obtain more important, and it is the research to absorbing material and coating to study electromangnetic spectrum most critical.Made using absorbing material
For the coating of electromangnetic spectrum, not only with low cost, technique is easy and can efficiently suppress electromagnetic pollution, therefore research performance
Excellent electromagnetic shielding material and absorbing material turn into the important topic that scientific research person studies
At present, the research both at home and abroad to absorbing material is concentrated mainly on following two aspects：Exploitation it is new there is wave absorbtion
The nano-powder of energy；Existing nano wave-absorbing material is doped or is combined, its absorbing property is improved and is carried
It is high.The shortcomings of above method has low efficiency, big frequency and big density simultaneously, these shortcomings make the application of absorbing material by one
Fixed limitation, therefore how to make high performance absorbing material and become developing direction.
The research to absorbing material requires that it should have at present：It is thin, light, wide, strong.I.e. thickness of thin, light weight, bandwidth,
Inhale the characteristics of ripple is strong.
Graphene is a kind of known most thin material, it is very rigid firmly, and, its strength ratio also stronger than diamond
It is also the performance being currently known most outstanding conductive material to taller hundred times best of steel, and its electronic movement velocity is
The 1/300 of the light velocity, the electronic movement velocity considerably beyond in general conductor, moreover, graphene thermal conductivity are good
(5000Wm-1K-1), the big (2630m of specific surface area2g-1), its Young's modulus (1100GPa) and fracture strength (125GPa) also may be used
Compared favourably with CNT.Graphene mainly plays dielectric loss to electromagnetic wave, but the electric conductivity of graphene is very good to be destroyed on the contrary
Impedance matching, declines its wave absorbtion.
Magnetic Nano material is the focus of modern absorbing material research, and magnetic nano-particle plays magnetic loss to electromagnetic wave
Effect, and excellent wave absorbtion is mainly shown in high frequency treatment.Due to haveing the shortcomings that easily to reunite, disperse nano-magnetic grain
Son is a difficult point.
In order that a greater degree of electromagnetic wave absorption of material, researchers are prepared into the material of dielectric loss and magnetic loss
Composite wave absorption material, the research of graphene composite material based on this is also a study hotspot now.
The content of the invention
The present invention provides a kind of preparation method of the graphene hollow microspheres of carried magnetic nano particle, and this method is to aoxidize
Graphene, polyvinyl alcohol and iron, cobalt, the metal salt of nickel are raw material, are prepared with water-in-oil inverse emulsion method a kind of uniform
It is loaded with the graphene oxide tiny balloon presoma of metal salt；And under protective atmosphere roasting reduction, obtain carried magnetic and receive
The graphene hollow microspheres of rice corpuscles.It this method solve graphene in the prior art and magnetic particle adhesion be not enough, magnetic
Particle is unable to uniform load on graphene, the problems such as magnetic particle is easily reunited.The graphite of the carried magnetic nano particle of preparation
The characteristics of alkene tiny balloon has high-specific surface area and low-density, is adjusted by the addition for adjusting metal salt and graphene oxide
Control the magnetic property and dielectric properties of microballoon.
In order to achieve the above object, technical solution of the present invention is：
A kind of preparation method of 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 instead by a certain percentage
Answer liquid；
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 includes methyl-silicone oil, dimethicone, soybean
One kind in oil, peanut oil, olive oil, Semen Benincasae oil, tea-seed oil, rapeseed oil and combinations thereof；Described metal salt includes levulinic
Ketone iron, nickel acetylacetonate, acetylacetone cobalt, cobalt nitrate, ferric nitrate, nickel nitrate, ferric acetate, cobalt acetate, nickel acetate, iron chloride,
One kind in nickel chloride, cobalt chloride and combinations thereof；Described liquid alcohols includes ethanol, methanol or the two mixture.
(2) 150-250ml oil is added in reaction vessel, heating water bath is to 60-75 DEG C；In 5000r/min-6000r/
The reaction solution for configuring step (1) under min mixing speed is slowly dropped into oil and stirred 5-10 minutes, forms the anti-of Water-In-Oil
Answer system；Mixing speed is down into 500-1000r/min to stir 3-5 hours；By warming-in-water to 90-100 DEG C, in 500-
Continue under 1000r/min mixing speed after stirring 3-5 hours；Finally by reacting liquid filtering, it is washed with deionized, in 60-
Dried under 80 DEG C of vacuum conditions, obtain being loaded with the graphene oxide tiny balloon presoma of metal salt.
(3) the graphene oxide tiny balloon presoma for obtaining step (2), the heating calcining 0.5-4 in protective atmosphere
Hour, cool to graphene oxide tiny balloon presoma with the furnace room temperature, that is, obtain the graphene of carried magnetic nano particle
Tiny balloon；
Described protection gas bag includes one kind of nitrogen, argon gas, neon, helium and combinations thereof, and protection air-flow amount is 40-
100ml/min；Described heating rate is 1-10 DEG C/min；Described calcining heat is 300-800 DEG C.
The graphene hollow microspheres material that prepared by the present invention be loaded with magnetic nano-particle has excellent electromagnetic performance, can
For electromagnetic wave absorbent material.
Beneficial effects of the present invention are：1. the graphene microballoon prepared is hollow, sphere diameter is 5-10 microns, by increasing capacitance it is possible to increase
The specific surface area of material, reduces the density of material, with specific surface area is high and the characteristics of small density, the surfaces externally and internally of microballoon and
Ball pars intramuralis is loaded with magnetic nano-particle；2. magnetic nano-particle is supported between graphene sheet layer, magnetic is not only solved
The problem of property nano-particle is reunited, while also solving the agglomeration traits of graphene in itself；3. by adjusting graphene and magnetic
The proportioning of nano-particle, adjusts the electromagnetic performance class of material, material has been widened significantly as wave-absorbing and camouflage and electromagnetic shielding
Effective frequency range during material.The graphene hollow microspheres material that prepared by the present invention be loaded with magnetic nano-particle has excellent electromagnetism
Performance, can be used for electromagnetic wave absorbent material.
Brief description of the drawings
Fig. 1 is load ferriferrous oxide nano-particle graphene microballoon surface sweeping electron microscope prepared by embodiment 2.
Fig. 2 is that embodiment 2 prepares load ferriferrous oxide nano-particle graphene microballoon minority because of sweeping that high temperature ruptures
Retouch electron microscope.
Fig. 3 is the microwave electromagnetic reflecting properties that embodiment 1-4 prepares load ferriferrous oxide nano-particle graphene microballoon
Test result figure.
Fig. 4 is the microwave for the simulation different-thickness that embodiment 2 prepares load ferriferrous oxide nano-particle graphene microballoon
ELECTROMAGNETIC REFLECTION the performance test results figure.
Embodiment
Embodiment 1：
Step 1：40mg graphene oxides are added in 50ml beaker, 7ml deionized waters, ultrasonically treated 30 is then added
Minute；Weigh 100mg polyvinyl alcohol to add in the mixed liquor of graphene oxide and water, stirring to polyvinyl alcohol is all dissolved, note
For A liquid.One, 50ml beakers are taken, 12ml ethanol is measured and adds in beaker, 200mg ferric acetyl acetonades is weighed and adds in beaker, stir
Mix to ferric acetyl acetonade and all dissolve, be designated as B liquid；A liquid and B liquid are mixed, and stirred, reaction solution is obtained.
Step 2：500ml there-necked flasks one are taken, 200ml olive oil is added, flask is put into 65 DEG C of water-baths and heated, and
Stirred using mixer, mixing speed is 5000r/min.The reaction solution that step 2 prepares is slowly added dropwise in flask, dripped
5min is persistently stirred under 5000r/min speed afterwards, mixing speed is then down to 500r/min, is persistently stirred 3 hours；Will
Water-bath rises to 90 DEG C, and continues stirring 3 hours under 500r/min rotating speeds, stops stirring afterwards；Filtering reacting liquid, uses deionization
Twice, last filter cake is dried in vacuo water cleaning filter cake at 70 DEG C, obtains loading ferric acetyl acetonade graphene oxide microballoon forerunner
Body.
Step 3：The load ferric acetyl acetonade graphene oxide microballoon that step 2 is obtained is put into crucible, and crucible is put into
In the quartz ampoule of tube furnace, argon gas is passed through into quartz ampoule, throughput is 50ml/min, after ventilating 20 minutes, stove starts to rise
Warm speed is 5 DEG C/min, and it is 400 DEG C to set calcining heat, and calcination time is 2 hours, cools to room temperature with the furnace afterwards, closes and protects
Gas is protected, the graphene hollow microspheres of carried magnetic nano particle are obtained.
Embodiment 2：
Step 1：50mg graphene oxides are added in 50ml beaker, 7ml deionized waters, ultrasonically treated 30 is then added
Minute；Weigh 200mg polyvinyl alcohol to add in the mixed liquor of graphene oxide and water, stirring to polyvinyl alcohol is all dissolved, note
For A liquid.One, 50ml beakers are taken, 15ml ethanol is measured and adds in beaker, 300mg ferric acetyl acetonades is weighed and adds in beaker, stir
Mix to ferric acetyl acetonade and all dissolve, be designated as B liquid；A liquid and B liquid are mixed, and stirred, reaction solution is obtained.
Step 2：500ml there-necked flasks one are taken, 200ml olive oil is added, flask is put into 70 DEG C of water-baths and heated, and
Stirred using mixer, mixing speed is 6000r/min.The reaction solution that step 2 prepares is slowly added dropwise in flask, dripped
10min is persistently stirred under 6000r/min speed afterwards, mixing speed is then down to 800r/min, is persistently stirred 4 hours；
Water-bath is risen to 95 DEG C, and continues stirring 4 hours under 800r/min rotating speeds, stops stirring afterwards；Filtering reacting liquid, spend from
Twice, last filter cake is dried in vacuo sub- water cleaning filter cake at 75 DEG C, is obtained before load ferric acetyl acetonade graphene oxide microballoon
Drive body.
Step 3：The load ferric acetyl acetonade graphene oxide microballoon that step 2 is obtained is put into crucible, and crucible is put into
In the quartz ampoule of tube furnace, argon gas is passed through into quartz ampoule, throughput is 60ml/min, after ventilating 20 minutes, stove starts to rise
Warm speed is 7 DEG C/min, and it is 500 DEG C to set calcining heat, and calcination time is 2 hours, cools to room temperature with the furnace afterwards, closes and protects
Gas is protected, the graphene hollow microspheres of carried magnetic nano particle are obtained.
Embodiment 3：
Step 1：70mg graphene oxides are added in 50ml beaker, 10ml deionized waters are then added, it is ultrasonically treated
30 minutes；Weigh 300mg polyvinyl alcohol to add in the mixed liquor of graphene oxide and water, stirring to polyvinyl alcohol is all dissolved,
It is designated as A liquid.One, 50ml beakers are taken, 20ml ethanol is measured and adds in beaker, 400mg ferric acetyl acetonades is weighed and adds in beaker,
Stirring is all dissolved to ferric acetyl acetonade, is designated as B liquid；A liquid and B liquid are mixed, and stirred, reaction solution is obtained.
Step 2：500ml there-necked flasks one are taken, 200ml olive oil is added, flask is put into 75 DEG C of water-baths and heated, and
Stirred using mixer, mixing speed is 6000r/min.The reaction solution that step 2 prepares is slowly added dropwise in flask, dripped
10min is persistently stirred under 6000r/min speed afterwards, mixing speed is then down to 1000r/min, is persistently stirred 5 hours；
Water-bath is risen to 100 DEG C, and continues stirring 5 hours under 1000r/min rotating speeds, stops stirring afterwards；Filtering reacting liquid, spends
Twice, last filter cake is dried in vacuo ionized water cleaning filter cake at 80 DEG C, obtains loading ferric acetyl acetonade graphene oxide microballoon
Presoma.
Step 3：The load ferric acetyl acetonade graphene oxide microballoon that step 2 is obtained is put into crucible, and crucible is put into
In the quartz ampoule of tube furnace, argon gas is passed through into quartz ampoule, throughput is 90ml/min, after ventilating 20 minutes, stove starts to rise
Warm speed is 10 DEG C/min, and it is 600 DEG C to set calcining heat, and calcination time is 4 hours, cools to room temperature with the furnace afterwards, is closed
Protective gas, obtains the graphene hollow microspheres of carried magnetic nano particle.
Embodiment 4：
Step 1：80mg graphene oxides are added in 50ml beaker, 10ml deionized waters are then added, it is ultrasonically treated
30 minutes；Weigh 300mg polyvinyl alcohol to add in the mixed liquor of graphene oxide and water, stirring to polyvinyl alcohol is all dissolved,
It is designated as A liquid.One, 50ml beakers are taken, 20ml ethanol is measured and adds in beaker, 400mg ferric acetyl acetonades is weighed and adds in beaker,
Stirring is all dissolved to ferric acetyl acetonade, is designated as B liquid；A liquid and B liquid are mixed, and stirred, reaction solution is obtained.
Step 2：500ml there-necked flasks one are taken, 200ml olive oil is added, flask is put into 75 DEG C of water-baths and heated, and
Stirred using mixer, mixing speed is 5000r/min.The reaction solution that step 2 prepares is slowly added dropwise in flask, dripped
5min is persistently stirred under 5000r/min speed afterwards, mixing speed is then down to 500r/min, is persistently stirred 3 hours；Will
Water-bath rises to 95 DEG C, and continues stirring 3 hours under 500r/min rotating speeds, stops stirring afterwards；Filtering reacting liquid, uses deionization
Twice, last filter cake is dried in vacuo water cleaning filter cake at 80 DEG C, obtains loading ferric acetyl acetonade graphene oxide microballoon forerunner
Body.
Step 3：The load ferric acetyl acetonade graphene oxide microballoon that step 2 is obtained is put into crucible, and crucible is put into
In the quartz ampoule of tube furnace, argon gas is passed through into quartz ampoule, throughput is 60ml/min, after ventilating 20 minutes, stove starts to rise
Warm speed is 5 DEG C/min, and it is 800 DEG C to set calcining heat, and calcination time is 4 hours, cools to room temperature with the furnace afterwards, closes and protects
Gas is protected, the graphene hollow microspheres of carried magnetic nano particle are obtained.
Claims (2)
1. a kind of preparation method of the graphene hollow microspheres of carried magnetic nano particle, it is characterised in that comprise the following steps：
(1) by 30-80mg graphene oxides, 6-10mL deionized waters, 12-22mL liquid alcohols, 100-300mg polyvinyl alcohol and
200-500mg metal salts are configured to reaction solution；Described liquid alcohols includes ethanol, methanol or the two mixture；
(2) 150-250ml oil is added in reaction vessel, heating water bath is to 60-75 DEG C；5000r/min-6000r/min's
Step (1) reaction solution is instilled in oil under mixing speed, stirred 5-10 minutes；Mixing speed is down into 500-1000r/min to stir
Mix 3-5 hours；By warming-in-water to 90-100 DEG C, it is stirred for 3-5 hours；Finally by reacting liquid filtering, it is washed with deionized
Vacuum drying obtains being loaded with the graphene oxide tiny balloon presoma of metal salt afterwards；
Described oil includes methyl-silicone oil, dimethicone, soybean oil, peanut oil, olive oil, Semen Benincasae oil, tea-seed oil, rapeseed oil
In one kind and combinations thereof；
Described metal salt includes ferric acetyl acetonade, nickel acetylacetonate, acetylacetone cobalt, cobalt nitrate, ferric nitrate, nickel nitrate, second
One kind in sour iron, cobalt acetate, nickel acetate, iron chloride, nickel chloride, cobalt chloride and combinations thereof；
(3) the graphene oxide tiny balloon presoma for obtaining step (2), is warming up in protective atmosphere by 1-10 DEG C/min
300-800 DEG C, calcine 0.5-4 hours；Cool to graphene oxide tiny balloon presoma with the furnace room temperature, obtain carried magnetic
The graphene hollow microspheres of nano-particle.
2. preparation method as claimed in claim 1, it is characterised in that described protection gas bag includes nitrogen, argon gas, neon, helium
One kind of gas and combinations thereof, protection air-flow amount is 40-100mL/min.
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| 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 |
| 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 |
| 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 |
| 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 |
| 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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| EP2939764B1 (en) * | 2012-12-27 | 2018-09-26 | LG Chem, Ltd. | Method for manufacturing hollow metal nanoparticle supported by support body |
| CN104479804A (en) * | 2014-11-25 | 2015-04-01 | 华南理工大学 | Nanometer copper/graphene composite material and preparation method and application thereof |
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