CN103641488B - Method for preparing graphene doped polyaniline-based carbon coated nickel zinc ferrite mesoporous material - Google Patents
Method for preparing graphene doped polyaniline-based carbon coated nickel zinc ferrite mesoporous material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 103
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 64
- 239000013335 mesoporous material Substances 0.000 title claims abstract description 36
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 title abstract description 7
- 239000002122 magnetic nanoparticle Substances 0.000 claims abstract description 51
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 38
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 104
- 238000002360 preparation method Methods 0.000 claims description 45
- 238000005406 washing Methods 0.000 claims description 40
- 239000011701 zinc Substances 0.000 claims description 40
- 239000010431 corundum Substances 0.000 claims description 35
- 229910052593 corundum Inorganic materials 0.000 claims description 35
- 239000011248 coating agent Substances 0.000 claims description 33
- 238000000576 coating method Methods 0.000 claims description 33
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 32
- 229910052759 nickel Inorganic materials 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000919 ceramic Substances 0.000 claims description 24
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 24
- 239000012286 potassium permanganate Substances 0.000 claims description 23
- 238000002485 combustion reaction Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 239000000178 monomer Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 11
- 239000003610 charcoal Substances 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 10
- 230000002776 aggregation Effects 0.000 claims description 9
- 238000004220 aggregation Methods 0.000 claims description 9
- 239000004160 Ammonium persulphate Substances 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000003837 high-temperature calcination Methods 0.000 claims description 8
- 238000010907 mechanical stirring Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 230000010355 oscillation Effects 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 206010013786 Dry skin Diseases 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 18
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- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
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- 238000010521 absorption reaction Methods 0.000 description 2
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- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- -1 graphite alkene Chemical class 0.000 description 1
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Abstract
The invention discloses a method for preparing a graphene doped polyaniline-based carbon coated nickel zinc ferrite mesoporous material, which combines conductive polymer polyaniline, ferrite and graphene material. The method comprises steps of firstly preparing a nickel zinc ferrite magnetic matrix through a self-propagating combustion method, then preparing graphene doped polyaniline coated nickel zinc ferrite magnetic nanoparticle through an in site polymerization method by taking graphene as the dopant, finally, carbonizing at high temperature and reducing so as to obtain the carbon coated graphene or nickel zinc ferrite nanometer mesoporous material. The graphene doped polyaniline-based carbon coated nickel zinc ferrite mesoporous material prepared by the method can be used as both an electromagnetic wave absorbing material and an environment adsorbing material for adsorbing pollutants such as heave metals, POPs (persistent organic pollutants) and the like in the environment, and has very important value in fields such as military stealth materials, electromagnetic shielding materials and environment adsorbing materials.
Description
Technical field
The present invention is a kind of preparation method of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material, belongs to electromagnetic shielding material, wave-absorbing and camouflage material and environment adsorbing materials field.
Background technology
Along with the fast development of the radar exploration technique, the probability that the military defense system of countries in the world and aircraft are detected by enemy, follow the tracks of and attack also promotes thereupon.For military target existence afield, defence and attacking ability, wave-absorbing and camouflage material also becomes the study hotspot of military technique.And along with the development of contemporary electronic information technology and the constantly universal of electronic product, electromagenetic wave radiation, while meeting people's life requirement, also result in the thorny problem such as electromagnetic pollution, electromagnetic interference, hampers the steady progression of electronic information industry.The research and development of electromagnetic shielding material are one of effective schemes solving electromagnetic radiation pollution.Traditional absorbing material has ferrite, graphite, conducting high polymers thing and the material such as ceramic-like and matrix material, its main drawback has density large, inhale the shortcomings such as ripple frequency band is narrow, be difficult to meet requirement that the stealthy and electronics of advanced weaponry equipment under modern battlefield condition runs well and can not be good meet the requirements such as absorbing material " thin, light, wide, strong ".
Summary of the invention
The object of this invention is to provide a kind of preparation method of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material, combine traditional conductive polymer polyanaline, ferrite and grapheme material.In the preparation, self-propagating combustion is first adopted to prepare nickel-zinc ferrite magnetic matrix, be doping agent again with Graphene, situ aggregation method is adopted to prepare the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline, the last above-mentioned magnetic nanoparticle of high temperature reduction carbonization again, obtains carbon coating graphite alkene/nickel-zinc ferrite mesoporous nano material.
A preparation method for Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material, concrete steps are as follows:
(1) self-propagating combustion prepares Ni
0.6zn
0.4fe
2o
4magnetic nanoparticle
Take 0.03mol Ni (NO
3)
26H
2o, 0.02mol Zn (NO
3)
26H
2o and 0.1molFe (NO
3)
39H
2o is dissolved in the there-necked flask that 100ml deionized water is housed, ultrasonic disperse, mixing, then add citric acid 0.1mol, regulate PH=7.0 with ammoniacal liquor, fast stirring 5min, mixture is gone to microwave oscillation in 65-75 DEG C of water-bath until the appearance of red-brown vitreosol, then colloidal sol to be transferred in thermostatic drying chamber 75-85 DEG C and to be dried to formation xerogel, drip 1-3ml dehydrated alcohol on xerogel, xerogel is placed in air light, self-propagating combustion can occurs and generate brown Ni
0.6zn
0.4fe
2o
4powder, finally puts into retort furnace 550-650 DEG C of calcining 5h, is cooled to room temperature, mills and obtain Powdered Ni by obtained powder
0.6zn
0.4fe
2o
4magnetic nanoparticle.
(2) preparation of Graphene
Take 2g graphite and be placed in 250ml beaker, add 10ml concentrated nitric acid, the 5ml vitriol oil, add 5g potassium permanganate again, ultrasonic disperse 10min, three times are washed with deionized water, add 5ml strong aqua and ultrasonic disperse 10min, after centrifuge washing 2 times, then add 10ml superoxol and ultrasonic disperse 10min, centrifuge washing 2 times, add 5ml concentrated hydrochloric acid and ultrasonic disperse 10min, wash twice, then add 10ml dehydrated alcohol and ultrasonic disperse 10min, filtering and washing three times, namely 90-110 DEG C of drying be prepared into Graphene.
(3) situ aggregation method prepares the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline
Take the Ni of the above-mentioned preparation of 1g
0.6zn
0.4fe
2o
4magnetic nanoparticle joins in 20 mL 1mol/L HCl solution, add ultrasonic disperse 10min after Graphene, add 2 mL aniline monomers again, the mass ratio of Graphene and aniline monomer is 1:0.5-1.5, mechanical stirring 10min forms A liquid, separately get a beaker, take 5g ammonium persulphate to be dissolved in 80 mL 1mol/L HCl solution and to form B liquid, ice bath limit, limit is stirred, while B liquid is dropwise joined in A liquid, after stirring 11-13 h, magnetic resolution throw out, and by deionized water filtering and washing and each three times of dehydrated alcohol filtering and washing, namely blackish green solid is prepared into the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline as after dry 22-26h at 75-85 DEG C.
(4) preparation of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material
The coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline taking the above-mentioned preparation of 1g is placed in high temperature cabonization reducing apparatus, taking 2g potassium permanganate is placed between corundum crucible and ceramic crucible, whole high temperature reduction device is placed in retort furnace high-temperature calcination, heating temperature curve is as follows: be raised to 900 DEG C and constant temperature 4h from room temperature, creep speed is 10 DEG C/min, when retort furnace is cooled to room temperature, magnetic resolution sample again, is namely prepared into Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material.
Above-mentioned High-temperature reduction carbonization device, is made up of corundum crucible lid, charcoal cake, ceramic crucible, potassium permanganate, corundum crucible; Ceramic crucible is enclosed within inside corundum crucible, and corundum crucible covers sealing by corundum crucible lid, and ceramic crucible is covered with by charcoal cake, between ceramic crucible and corundum crucible, be evenly covered with potassium permanganate.
The typical sizes of all parts is as follows:
Corundum crucible: it is 6cm that corundum crucible makes external diameter by aluminium sesquioxide calcining, and external diameter is 5cm, high 8cm, the hollow circular cylinder shape corundum crucible of base thickness 1cm.
Corundum crucible lid: it is 6cm that corundum crucible lid makes diameter by aluminium sesquioxide calcining, the cylindric corundum crucible lid of high 0.8cm, for covering corundum crucible, stops the gas overflowing in corundum crucible chamber.This corundum crucible lid also useful ceramics crucible replaces.
Ceramic crucible: ceramic crucible is internal diameter is 3.65cm, the conventional ceramic crucible of external diameter 4.2cm, needs material to be processed for holding.
Charcoal cake: it is 4.7cm that charcoal cake is pressed into diameter by active carbon powder, the cylindrical shape charcoal cake of high 0.8cm, in order to provide reductive agent.Charcoal cake surface irregularity, can allow the gas in corundum crucible enter ceramic crucible inside, with materials from oxidizing reduction reaction when covering on ceramic crucible.
Potassium permanganate: the character of material to be processed is different with quality according to needing, and the quality being laid in the potassium permanganate bottom corundum crucible is also different.
Carbonaceous material is the important content that electromagnetic shielding and absorbing material are studied as carbon black, graphite, carbon nanotube and carbon fiber always, has had and has studied quite widely.Graphene, compared with traditional absorbing material, has the physicochemical property of following uniqueness: the sexangle two-dimensional material that (1) Graphene is made up of carbon atom, only has the thickness of a carbon atom; (2) thermal conductivity reaches 5300W/mk, higher than carbon nanotube and diamond; (3) resistivity of Graphene reaches 10
-6Ω cm is one of material that current resistivity is minimum; (4) Graphene is nano material the thinnest and the hardest in the world at present; (5) under normal temperature Graphene electronic mobility more than 15000cm
2/ Vs, exceedes the electronic mobility of carbon nanotube.Thus Graphene becomes the focus of research electromagnetic-wave absorbent.
Ferrite is traditional absorbing material of a kind of pair of composite dielectric, there is magnetic loss and dielectric loss two kinds effect simultaneously, thus have good absorbing property to hertzian wave.Ferrite wave-absorbing material has the advantages, particularly M ferrite such as absorption frequency range is high, specific absorption is high, matching thickness is thin have received numerous researcher favor because it has higher magnetocrystalline anisotropy.
Polyaniline is a kind of conductive polymers, has good electroconductibility and environmental stability and cause the extensive concern of every field because of it.Conductive polymer polyanaline has large conjugatedπbond, carries out doping and polyaniline specific conductivity at room temperature can be made between isolator, between semi-conductor and the specific conductivity of metal, thus show excellent physics-chem characteristic by diverse ways to conjugated chain.
Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material prepared by the present invention has excellent performance, good size, higher specific conductivity and the maximum suction ripple within the scope of 1-20Hz, there is important using value, can be used for electromagnetic-wave absorbent, environment adsorbing materials can be used as again, for adsorbing in environment as the pollutent such as heavy metal, POPs.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Description of reference numerals: corundum crucible lid 1, charcoal cake 2, ceramic crucible 3, potassium permanganate 4, corundum crucible 5.
Embodiment
Embodiment 1:
A preparation method for Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material, concrete steps are as follows:
(1) self-propagating combustion prepares Ni
0.6zn
0.4fe
2o
4magnetic nanoparticle
Take 0.03mol Ni (NO
3)
26H
2o, 0.02mol Zn (NO
3)
26H
2o and 0.1molFe (NO
3)
39H
2o is dissolved in the there-necked flask that 100ml deionized water is housed, ultrasonic disperse, mixing, then add citric acid 0.1mol, regulate PH=7.0 with ammoniacal liquor, fast stirring 5min, mixture is gone to microwave oscillation in 65 DEG C of water-baths until the appearance of red-brown vitreosol, then colloidal sol to be transferred in thermostatic drying chamber 75 DEG C and to be dried to formation xerogel, drip 1ml dehydrated alcohol on xerogel, xerogel is placed in air light, self-propagating combustion can occurs and generate brown Ni
0.6zn
0.4fe
2o
4powder, finally puts into retort furnace 550 DEG C calcining 5h, is cooled to room temperature, mills and obtain Powdered Ni by obtained powder
0.6zn
0.4fe
2o
4magnetic nanoparticle.
(2) preparation of Graphene
Take 2g graphite and be placed in 250ml beaker, add 10ml concentrated nitric acid, the 5ml vitriol oil, add 5g potassium permanganate again, ultrasonic disperse 10min, three times are washed with deionized water, add 5ml strong aqua and ultrasonic disperse 10min, after centrifuge washing 2 times, then add 10ml superoxol and ultrasonic disperse 10min, centrifuge washing 2 times, add 5ml concentrated hydrochloric acid and ultrasonic disperse 10min, wash twice, then add 10ml dehydrated alcohol and ultrasonic disperse 10min, filtering and washing three times, namely 90 DEG C of dryings are prepared into Graphene.
(3) situ aggregation method prepares the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline
Take the Ni of the above-mentioned preparation of 1g
0.6zn
0.4fe
2o
4magnetic nanoparticle joins in 20 mL 1mol/L HCl solution, add ultrasonic disperse 10min after Graphene, add 2 mL aniline monomers again, the mass ratio of Graphene and aniline monomer is 1:0.5, mechanical stirring 10min forms A liquid, separately get a beaker, take 5g ammonium persulphate to be dissolved in 80 mL 1mol/L HCl solution and to form B liquid, ice bath limit, limit is stirred, while B liquid is dropwise joined in A liquid, after stirring 11h, magnetic resolution throw out, and by deionized water filtering and washing and each three times of dehydrated alcohol filtering and washing, namely blackish green solid is prepared into the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline as after dry 22h at 75 DEG C.
(4) preparation of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material
The coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline taking the above-mentioned preparation of 1g is placed in high temperature cabonization reducing apparatus, taking 2g potassium permanganate is placed between corundum crucible and ceramic crucible, whole high temperature reduction device is placed in retort furnace high-temperature calcination, heating temperature curve is as follows: be raised to 900 DEG C and constant temperature 4h from room temperature, creep speed is 10 DEG C/min, when retort furnace is cooled to room temperature, magnetic resolution sample again, is namely prepared into Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material.
Embodiment 2:
A preparation method for Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material, concrete steps are as follows:
(1) self-propagating combustion prepares Ni
0.6zn
0.4fe
2o
4magnetic nanoparticle
Take 0.03mol Ni (NO
3)
26H
2o, 0.02mol Zn (NO
3)
26H
2o and 0.1molFe (NO
3)
39H
2o is dissolved in the there-necked flask that 100ml deionized water is housed, ultrasonic disperse, mixing, then add citric acid 0.1mol, regulate PH=7.0 with ammoniacal liquor, fast stirring 5min, mixture is gone to microwave oscillation in 70 DEG C of water-baths until the appearance of red-brown vitreosol, then colloidal sol to be transferred in thermostatic drying chamber 80 DEG C and to be dried to formation xerogel, drip 2ml dehydrated alcohol on xerogel, xerogel is placed in air light, self-propagating combustion can occurs and generate brown Ni
0.6zn
0.4fe
2o
4powder, finally puts into retort furnace 600 DEG C calcining 5h, is cooled to room temperature, mills and obtain Powdered Ni by obtained powder
0.6zn
0.4fe
2o
4magnetic nanoparticle.
(2) preparation of Graphene
Take 2g graphite and be placed in 250ml beaker, add 10ml concentrated nitric acid, the 5ml vitriol oil, add 5g potassium permanganate again, ultrasonic disperse 10min, three times are washed with deionized water, add 5ml strong aqua and ultrasonic disperse 10min, after centrifuge washing 2 times, then add 10ml superoxol and ultrasonic disperse 10min, centrifuge washing 2 times, add 5ml concentrated hydrochloric acid and ultrasonic disperse 10min, wash twice, then add 10ml dehydrated alcohol and ultrasonic disperse 10min, filtering and washing three times, namely 100 DEG C of dryings are prepared into Graphene.
(3) situ aggregation method prepares the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline
Take the Ni of the above-mentioned preparation of 1g
0.6zn
0.4fe
2o
4magnetic nanoparticle joins in 20 mL 1mol/L HCl solution, add ultrasonic disperse 10min after Graphene, add 2 mL aniline monomers again, the mass ratio of Graphene and aniline monomer is 1:1, mechanical stirring 10min forms A liquid, separately get a beaker, take 5g ammonium persulphate to be dissolved in 80 mL 1mol/L HCl solution and to form B liquid, ice bath limit, limit is stirred, while B liquid is dropwise joined in A liquid, after stirring 12 h, magnetic resolution throw out, and by deionized water filtering and washing and each three times of dehydrated alcohol filtering and washing, namely blackish green solid is prepared into the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline as after dry 24h at 80 DEG C.
(4) preparation of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material
The coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline taking the above-mentioned preparation of 1g is placed in high temperature cabonization reducing apparatus, taking 2g potassium permanganate is placed between corundum crucible and ceramic crucible, whole high temperature reduction device is placed in retort furnace high-temperature calcination, heating temperature curve is as follows: be raised to 900 DEG C and constant temperature 4h from room temperature, creep speed is 10 DEG C/min, when retort furnace is cooled to room temperature, magnetic resolution sample again, is namely prepared into Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material.
Embodiment 3:
A preparation method for Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material, concrete steps are as follows:
(1) self-propagating combustion prepares Ni
0.6zn
0.4fe
2o
4magnetic nanoparticle
Take 0.03mol Ni (NO
3)
26H
2o, 0.02mol Zn (NO
3)
26H
2o and 0.1molFe (NO
3)
39H
2o is dissolved in the there-necked flask that 100ml deionized water is housed, ultrasonic disperse, mixing, then add citric acid 0.1mol, regulate PH=7.0 with ammoniacal liquor, fast stirring 5min, mixture is gone to microwave oscillation in 75 DEG C of water-baths until the appearance of red-brown vitreosol, then colloidal sol to be transferred in thermostatic drying chamber 85 DEG C and to be dried to formation xerogel, drip 3ml dehydrated alcohol on xerogel, xerogel is placed in air light, self-propagating combustion can occurs and generate brown Ni
0.6zn
0.4fe
2o
4powder, finally puts into retort furnace 650 DEG C calcining 5h, is cooled to room temperature, mills and obtain Powdered Ni by obtained powder
0.6zn
0.4fe
2o
4magnetic nanoparticle.
(2) preparation of Graphene
Take 2g graphite and be placed in 250ml beaker, add 10ml concentrated nitric acid, the 5ml vitriol oil, add 5g potassium permanganate again, ultrasonic disperse 10min, three times are washed with deionized water, add 5ml strong aqua and ultrasonic disperse 10min, after centrifuge washing 2 times, then add 10ml superoxol and ultrasonic disperse 10min, centrifuge washing 2 times, add 5ml concentrated hydrochloric acid and ultrasonic disperse 10min, wash twice, then add 10ml dehydrated alcohol and ultrasonic disperse 10min, filtering and washing three times, namely 110 DEG C of dryings are prepared into Graphene.
(3) situ aggregation method prepares the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline
Take the Ni of the above-mentioned preparation of 1g
0.6zn
0.4fe
2o
4magnetic nanoparticle joins in 20 mL 1mol/L HCl solution, add ultrasonic disperse 10min after Graphene, add 2 mL aniline monomers again, the mass ratio of Graphene and aniline monomer is 1:1.5, mechanical stirring 10min forms A liquid, separately get a beaker, take 5g ammonium persulphate to be dissolved in 80 mL 1mol/L HCl solution and to form B liquid, ice bath limit, limit is stirred, while B liquid is dropwise joined in A liquid, after stirring 13 h, magnetic resolution throw out, and by deionized water filtering and washing and each three times of dehydrated alcohol filtering and washing, namely blackish green solid is prepared into the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline as after dry 26h at 85 DEG C.
(4) preparation of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material
The coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline taking the above-mentioned preparation of 1g is placed in high temperature cabonization reducing apparatus, taking 2g potassium permanganate is placed between corundum crucible and ceramic crucible, whole high temperature reduction device is placed in retort furnace high-temperature calcination, heating temperature curve is as follows: be raised to 900 DEG C and constant temperature 4h from room temperature, creep speed is 10 DEG C/min, when retort furnace is cooled to room temperature, magnetic resolution sample again, is namely prepared into Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material.
Embodiment 4:
A preparation method for Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material, concrete steps are as follows:
(1) self-propagating combustion prepares Ni
0.6zn
0.4fe
2o
4magnetic nanoparticle
Take 0.03mol Ni (NO
3)
26H
2o, 0.02mol Zn (NO
3)
26H
2o and 0.1molFe (NO
3)
39H
2o is dissolved in the there-necked flask that 100ml deionized water is housed, ultrasonic disperse, mixing, then add citric acid 0.1mol, regulate PH=7.0 with ammoniacal liquor, fast stirring 5min, mixture is gone to microwave oscillation in 60 DEG C of water-baths until the appearance of red-brown vitreosol, then colloidal sol to be transferred in thermostatic drying chamber 70 DEG C and to be dried to formation xerogel, drip 1ml dehydrated alcohol on xerogel, xerogel is placed in air light, self-propagating combustion can occurs and generate brown Ni
0.6zn
0.4fe
2o
4powder, finally puts into retort furnace 500 DEG C calcining 5h, is cooled to room temperature, mills and obtain Powdered Ni by obtained powder
0.6zn
0.4fe
2o
4magnetic nanoparticle.
(2) preparation of Graphene
Take 2g graphite and be placed in 250ml beaker, add 10ml concentrated nitric acid, the 5ml vitriol oil, add 5g potassium permanganate again, ultrasonic disperse 10min, three times are washed with deionized water, add 5ml strong aqua and ultrasonic disperse 10min, after centrifuge washing 2 times, then add 10ml superoxol and ultrasonic disperse 10min, centrifuge washing 2 times, add 5ml concentrated hydrochloric acid and ultrasonic disperse 10min, wash twice, then add 10ml dehydrated alcohol and ultrasonic disperse 10min, filtering and washing three times, namely 85 DEG C of dryings are prepared into Graphene.
(3) situ aggregation method prepares the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline
Take the Ni of the above-mentioned preparation of 1g
0.6zn
0.4fe
2o
4magnetic nanoparticle joins in 20 mL 1mol/L HCl solution, add ultrasonic disperse 10min after Graphene, add 2 mL aniline monomers again, the mass ratio of Graphene and aniline monomer is 1:0.4, mechanical stirring 10min forms A liquid, separately get a beaker, take 5g ammonium persulphate to be dissolved in 80 mL 1mol/L HCl solution and to form B liquid, ice bath limit, limit is stirred, while B liquid is dropwise joined in A liquid, after stirring 10 h, magnetic resolution throw out, and by deionized water filtering and washing and each three times of dehydrated alcohol filtering and washing, namely blackish green solid is prepared into the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline as after dry 20h at 70 DEG C.
(4) preparation of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material
The coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline taking the above-mentioned preparation of 1g is placed in high temperature cabonization reducing apparatus, taking 2g potassium permanganate is placed between corundum crucible and ceramic crucible, whole high temperature reduction device is placed in retort furnace high-temperature calcination, heating temperature curve is as follows: be raised to 900 DEG C and constant temperature 4h from room temperature, creep speed is 10 DEG C/min, when retort furnace is cooled to room temperature, magnetic resolution sample again, is namely prepared into Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material.
Embodiment 5:
A preparation method for Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material, concrete steps are as follows:
(1) self-propagating combustion prepares Ni
0.6zn
0.4fe
2o
4magnetic nanoparticle
Take 0.03mol Ni (NO
3)
26H
2o, 0.02mol Zn (NO
3)
26H
2o and 0.1molFe (NO
3)
39H
2o is dissolved in the there-necked flask that 100ml deionized water is housed, ultrasonic disperse, mixing, then add citric acid 0.1mol, regulate PH=7.0 with ammoniacal liquor, fast stirring 5min, mixture is gone to microwave oscillation in 80 DEG C of water-baths until the appearance of red-brown vitreosol, then colloidal sol to be transferred in thermostatic drying chamber 90 DEG C and to be dried to formation xerogel, drip 4ml dehydrated alcohol on xerogel, xerogel is placed in air light, self-propagating combustion can occurs and generate brown Ni
0.6zn
0.4fe
2o
4powder, finally puts into retort furnace 700 DEG C calcining 5h, is cooled to room temperature, mills and obtain Powdered Ni by obtained powder
0.6zn
0.4fe
2o
4magnetic nanoparticle.
(2) preparation of Graphene
Take 2g graphite and be placed in 250ml beaker, add 10ml concentrated nitric acid, the 5ml vitriol oil, add 5g potassium permanganate again, ultrasonic disperse 10min, three times are washed with deionized water, add 5ml strong aqua and ultrasonic disperse 10min, after centrifuge washing 2 times, then add 10ml superoxol and ultrasonic disperse 10min, centrifuge washing 2 times, add 5ml concentrated hydrochloric acid and ultrasonic disperse 10min, wash twice, then add 10ml dehydrated alcohol and ultrasonic disperse 10min, filtering and washing three times, namely 120 DEG C of dryings are prepared into Graphene.
(3) situ aggregation method prepares the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline
Take the Ni of the above-mentioned preparation of 1g
0.6zn
0.4fe
2o
4magnetic nanoparticle joins in 20 mL 1mol/L HCl solution, add ultrasonic disperse 10min after Graphene, add 2 mL aniline monomers again, the mass ratio of Graphene and aniline monomer is 1:1.6, mechanical stirring 10min forms A liquid, separately get a beaker, take 5g ammonium persulphate to be dissolved in 80 mL 1mol/L HCl solution and to form B liquid, ice bath limit, limit is stirred, while B liquid is dropwise joined in A liquid, after stirring 15 h, magnetic resolution throw out, and by deionized water filtering and washing and each three times of dehydrated alcohol filtering and washing, namely blackish green solid is prepared into the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline as after dry 28h at 90 DEG C.
(4) preparation of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material
The coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline taking the above-mentioned preparation of 1g is placed in high temperature cabonization reducing apparatus, taking 2g potassium permanganate is placed between corundum crucible and ceramic crucible, whole high temperature reduction device is placed in retort furnace high-temperature calcination, heating temperature curve is as follows: be raised to 900 DEG C and constant temperature 4h from room temperature, creep speed is 10 DEG C/min, when retort furnace is cooled to room temperature, magnetic resolution sample again, is namely prepared into Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material.
The Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material TEM test result that each embodiment obtains is as shown in the table:
| Mesoporous nano scantling | Specific conductivity | Maximum suction ripple within the scope of 1-20Hz | |
| Embodiment 1 | 20nm | 1.813 S/cm | -45dB |
| Embodiment 2 | 18nm | 2.393 S/cm, | -48dB |
| Embodiment 3 | 22nm | 2.145 S/cm | -47dB |
| Embodiment 4 | 30nm | 1.267 S/cm | -31dB |
| Embodiment 5 | 28nm | 1.186 S/cm | -34dB |
As can be seen from the above data, the performance that embodiment 1-3 within the scope of present invention process obtains Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material is obviously better than in the extraneous embodiment 4,5 of present invention process, especially with the best results of embodiment 2, Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material prepared by the visible the present invention of have employed has good size, higher specific conductivity and the maximum suction ripple within the scope of 1-20Hz, have important using value.
Claims (3)
1. a preparation method for Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material, is characterized by: concrete steps are as follows:
(1) self-propagating combustion prepares Ni
0.6zn
0.4fe
2o
4magnetic nanoparticle
Take 0.03mol Ni (NO
3)
26H
2o, 0.02mol Zn (NO
3)
26H
2o and 0.1molFe (NO
3)
39H
2o is dissolved in the there-necked flask that 100ml deionized water is housed, ultrasonic disperse, mixing, then add citric acid 0.1mol, regulate PH=7.0 with ammoniacal liquor, fast stirring 5min, mixture is gone to microwave oscillation in 65-75 DEG C of water-bath until the appearance of red-brown vitreosol, then colloidal sol to be transferred in thermostatic drying chamber 75-85 DEG C and to be dried to formation xerogel, drip 1-3ml dehydrated alcohol on xerogel, xerogel is placed in air light, self-propagating combustion can occurs and generate brown Ni
0.6zn
0.4fe
2o
4powder, finally puts into retort furnace 550-650 DEG C of calcining 5h, is cooled to room temperature, mills and obtain Powdered Ni by obtained powder
0.6zn
0.4fe
2o
4magnetic nanoparticle;
(2) preparation of Graphene
Take 2g graphite and be placed in 250ml beaker, add 10ml concentrated nitric acid, the 5ml vitriol oil, add 5g potassium permanganate again, ultrasonic disperse 10min, three times are washed with deionized water, add 5ml strong aqua and ultrasonic disperse 10min, after centrifuge washing 2 times, then add 10ml superoxol and ultrasonic disperse 10min, centrifuge washing 2 times, add 5ml concentrated hydrochloric acid and ultrasonic disperse 10min, wash twice, then add 10ml dehydrated alcohol and ultrasonic disperse 10min, filtering and washing three times, namely 90-110 DEG C of drying be prepared into Graphene;
(3) situ aggregation method prepares the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline
Take the Ni of the above-mentioned preparation of 1g
0.6zn
0.4fe
2o
4magnetic nanoparticle joins in 20 mL 1mol/L HCl solution, add ultrasonic disperse 10min after Graphene, add 2 mL aniline monomers again, the mass ratio of Graphene and aniline monomer is 1:0.5-1.5, mechanical stirring 10min forms A liquid, separately get a beaker, take 5g ammonium persulphate to be dissolved in 80 mL 1mol/L HCl solution and to form B liquid, ice bath limit, limit is stirred, while B liquid is dropwise joined in A liquid, after stirring 11-13 h, magnetic resolution throw out, and by deionized water filtering and washing and each three times of dehydrated alcohol filtering and washing, namely blackish green solid is prepared into the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline as after dry 22-26h at 75-85 DEG C,
(4) preparation of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material
The coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline taking the above-mentioned preparation of 1g is placed in high temperature cabonization reducing apparatus, taking 2g potassium permanganate is placed between corundum crucible and ceramic crucible, whole high temperature reduction device is placed in retort furnace high-temperature calcination, heating temperature curve is as follows: be raised to 900 DEG C and constant temperature 4h from room temperature, creep speed is 10 DEG C/min, when retort furnace is cooled to room temperature, magnetic resolution sample again, is namely prepared into Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material.
2. the preparation method of a kind of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material as claimed in claim 1, is characterized by: concrete steps are as follows:
(1) self-propagating combustion prepares Ni
0.6zn
0.4fe
2o
4magnetic nanoparticle
Take 0.03mol Ni (NO
3)
26H
2o, 0.02mol Zn (NO
3)
26H
2o and 0.1molFe (NO
3)
39H
2o is dissolved in the there-necked flask that 100ml deionized water is housed, ultrasonic disperse, mixing, then add citric acid 0.1mol, regulate PH=7.0 with ammoniacal liquor, fast stirring 5min, mixture is gone to microwave oscillation in 70 DEG C of water-baths until the appearance of red-brown vitreosol, then colloidal sol to be transferred in thermostatic drying chamber 80 DEG C and to be dried to formation xerogel, drip 2ml dehydrated alcohol on xerogel, xerogel is placed in air light, self-propagating combustion can occurs and generate brown Ni
0.6zn
0.4fe
2o
4powder, finally puts into retort furnace 600 DEG C calcining 5h, is cooled to room temperature, mills and obtain Powdered Ni by obtained powder
0.6zn
0.4fe
2o
4magnetic nanoparticle;
(2) preparation of Graphene
Take 2g graphite and be placed in 250ml beaker, add 10ml concentrated nitric acid, the 5ml vitriol oil, add 5g potassium permanganate again, ultrasonic disperse 10min, three times are washed with deionized water, add 5ml strong aqua and ultrasonic disperse 10min, after centrifuge washing 2 times, then add 10ml superoxol and ultrasonic disperse 10min, centrifuge washing 2 times, add 5ml concentrated hydrochloric acid and ultrasonic disperse 10min, wash twice, then add 10ml dehydrated alcohol and ultrasonic disperse 10min, filtering and washing three times, namely 100 DEG C of dryings are prepared into Graphene;
(3) situ aggregation method prepares the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline
Take the Ni of the above-mentioned preparation of 1g
0.6zn
0.4fe
2o
4magnetic nanoparticle joins in 20 mL 1mol/L HCl solution, add ultrasonic disperse 10min after Graphene, add 2 mL aniline monomers again, the mass ratio of Graphene and aniline monomer is 1:1, mechanical stirring 10min forms A liquid, separately get a beaker, take 5g ammonium persulphate to be dissolved in 80 mL 1mol/L HCl solution and to form B liquid, ice bath limit, limit is stirred, while B liquid is dropwise joined in A liquid, after stirring 12 h, magnetic resolution throw out, and by deionized water filtering and washing and each three times of dehydrated alcohol filtering and washing, namely blackish green solid is prepared into the coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline as after dry 24h at 80 DEG C,
(4) preparation of Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material
The coated nickel-zinc ferrite magnetic nanoparticle of Graphene doped polyaniline taking the above-mentioned preparation of 1g is placed in high temperature cabonization reducing apparatus, taking 2g potassium permanganate is placed between corundum crucible and ceramic crucible, whole high temperature reduction device is placed in retort furnace high-temperature calcination, heating temperature curve is as follows: be raised to 900 DEG C and constant temperature 4h from room temperature, creep speed is 10 DEG C/min, when retort furnace is cooled to room temperature, magnetic resolution sample again, is namely prepared into Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material.
3. the preparation method planting Graphene doped polyaniline base carbon-coating nickel Zn ferrite mesoporous material as claimed in claim 1 or 2, is characterized by: high temperature cabonization reducing apparatus is made up of corundum crucible lid (1), charcoal cake (2), ceramic crucible (3), potassium permanganate (4), corundum crucible (5); Ceramic crucible (3) is enclosed within corundum crucible (5) the inside, corundum crucible (5) covers sealing by corundum crucible lid (1), ceramic crucible (3) is covered with by charcoal cake (2), is evenly covered with potassium permanganate (4) between ceramic crucible (3) and corundum crucible (5);
It is 6cm that corundum crucible (5) makes external diameter by aluminium sesquioxide calcining, and internal diameter is 5cm, high 8cm, the hollow circular cylinder shape of base thickness 1cm;
It is 6cm that corundum crucible lid (1) makes diameter by aluminium sesquioxide calcining, and high 0.8cm's is cylindric;
Ceramic crucible (3) for internal diameter be 3.65cm, external diameter 4.2cm;
Charcoal cake (2) is pressed into by active carbon powder the cylindrical shape that diameter is 4.7cm, high 0.8cm, surface irregularity.
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| CN105880614A (en) * | 2015-01-12 | 2016-08-24 | 冯云 | Mesoporous material with nano nickel loaded on graphene |
| CN104789188A (en) * | 2015-01-12 | 2015-07-22 | 冯云 | A preparing method of a nanometer mesoporous material |
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| CN104762060A (en) * | 2015-02-28 | 2015-07-08 | 冯云 | Preparation method for mesoporous material |
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