CN101941842A - Method for preparing graphene loaded ferroferric oxide magnetic nanometer particle composite material - Google Patents
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Abstract
The invention relates to a method for preparing a graphene loaded ferroferric oxide magnetic nanometer particle composite material. The method comprises the following steps of: (1) dispersing graphite oxide into deionized water, pouring into a vessel after ultrasonic and centrifuging, putting the vessel into an oil-bath pan, adding hydrazine hydrate and an anionic surfactant for heating, condensing and refluxing, and cooling and drying to obtain modified graphene; and (2) dispersing the graphene into aqueous solution, and ultrasonically stirring and centrifuging to obtain modified graphene dispersion liquid; and weighing a soluble trivalent ferric salt and divalent ferric salt, dissolving the salt into the deionized water, introducing nitrogen, pouring into the modified graphene dispersion liquid, dripping ammonia after uniform ultrasonic stirring, heating for reaction, washing and collecting a product, and drying the product. The method is simple and easy for industrial production; and the prepared composite material has the advantages of pure crystal phase, uniform distribution and excellent electrocatalytic activity.
Description
Technical field
The invention belongs to the preparation field of ferroferric oxide magnetic nanoparticle matrix material, particularly relate to a kind of preparation method of graphene-supported ferroferric oxide magnetic nanoparticle matrix material.
Background technology
Graphene is a kind of carbonaceous novel material by the tightly packed one-tenth bi-dimensional cellular of monolayer carbon atom shape crystalline network, it is the elementary cell that makes up zero dimension soccerballene, one dimension carbon nanotube, three-dimensional graphite, its excellent electricity, calorifics, mechanics and chemical property, be expected in the acquisition widespread use of fields such as high-performance nanometer electronic device, matrix material, field emmision material, electrochemical sensor and energy storage, therefore, since Geim in 2004 found Graphene, Graphene became one of the research focus in Materials science and Condensed Matter Physics field rapidly.With respect to other dimension carbonaceous materials, Graphene has the advantage of highly significant, it has excellent conducting performance and the chemical property except the same with carbon nanotube, it is cheap also to have preparation cost, technology simply and not can be introduced advantages such as other impurity, therefore we make corresponding research to Graphene and have very important significance based on the applied research of carbon nanotube, and wherein the application of Graphene aspect electrochemistry just has been subjected to scientific worker's extensive concern.
Graphene is a kind of good electrode materials, and its application aspect electrochemical sensor has demonstrated good performance and use prospect.People such as Longhua Tang have reported the chemical property of the graphene film of chemical reduction on [Advanced Functional Materials 19 (2009) 1-8], result of study shows that graphene-based electrode materials has higher electric transmission speed and outstanding electro catalytic activity, has confirmed the potential application of Graphene in biosensor, energy transformation and other electronic systems.People such as Ming Zhou have proposed a new electrode system at [Analytical Chemistry 81 (2009) 5603-5613], it is the graphene oxide/glass-carbon electrode (CR-GO/GC) of chemical reduction, result of study shows that the CR-GO/GC electrode can be widely used in Enzyme sensor and unmarked DNA transmitter, this research widened CR-GO with and hybrid material in the application aspect electroanalytical chemistry and the transmitter.This shows that the application aspect electrochemistry of Graphene and matrix material thereof has very wide significance.
Fe
3O
4Magnetic nanoparticle is because its special physicochemical character has application widely at aspects such as magnetic liquid, magnetic recording material, catalysis, biomedicine, microwave absorbing materials.There is report to confirm Fe at present again
3O
4Magnetic nanoparticle has the activity of similar superoxide, can be used as a kind of superoxide analogue enztme and substitutes natural enzyme, solves natural enzyme volatility, easily degraded, prepares the shortcoming that purifying is wasted time and energy.People such as Hui Wei have reported Fe at [Analytical Chemistry 80 (2008) 2250-2254]
3O
4The application of magnetic nanoparticle in hydrogen peroxide and glucose detection.People such as Qing Chang have reported Fe too on [Microchim Acta 165 (2009) 299-305]
3O
4The similar Peroxidase activity that magnetic nanoparticle shows hydrogen peroxide, Fe in addition
3O
4Because himself is nontoxic and with low cost, thereby thought one of electrode materials of potentialization by everybody.
In sum, to have the matrix of good electrical chemical property and have the active magnetic nanoparticle of superoxide analogue enztme and assemble, the matrix material for preparing has better electro catalytic activity, and this material can utilize the effect of externally-applied magnetic field to extract recycling.People such as Song Qu have reported carbon nanotube/nano Fe at [Talanta 71 (2007) 1096-1102]
3O
4Matrix material as electrode materials in the application aspect the electrochemical sensor, result of study shows that the adding of carbon nanotube has improved electrode materials to the electro catalytic activity of hydrogen peroxide in redox processes.People such as Xiaolei Zuo have reported equally that at [Nano Research 2 (2009) 617-623] carbon nanotube/magnetic nanoparticle matrix material is to the application aspect the efficiently catalyzing and oxidizing of phenolic compound.At this, we utilize Graphene to replace carbon nanotube as matrix, and the Graphene with the SDS modification is that raw material adopts chemical precipitation method to prepare the graphene-based nano composite material with good electrical catalytic activity first.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of graphene-supported ferroferric oxide magnetic nanoparticle matrix material, and this method is simple, is easy to suitability for industrialized production; Prepared matrix material crystalline phase is pure, be evenly distributed, and electro catalytic activity is good.
The preparation method of a kind of graphene-supported ferroferric oxide magnetic nanoparticle matrix material of the present invention comprises:
(1) modification of Graphene
Taking by weighing 200～240mg graphite oxide is scattered in the deionized water of 200～240ml, ultrasonic 60～100min, pour in the container behind the centrifugal removal macrobead, container is put into oil bath pan, add the hydrazine hydrate of 2～3ml and the anion surfactant of 0.1～0.2g, be heated to 100～120 ℃, condensing reflux 20～24 hours is cooled to the Graphene that oven dry after the room temperature obtains modification;
(2) chemical precipitation method prepares graphene-supported ferroferric oxide magnetic nanoparticle matrix material
The Graphene that takes by weighing above-mentioned modification is scattered in the aqueous solution, ultrasonic agitation, and centrifugal removal macrobead gets the Graphene dispersion liquid of modification; Take by weighing solubility trivalent iron salt and divalent iron salt, be dissolved in deionized water, feed nitrogen 10～30min, pour into then in the Graphene dispersion liquid of described modification, after ultrasonic agitation is even, dropping ammonia, dropping is heated to 50～70 ℃ with mixed solution after finishing, reaction 30～60min, question response finishes postcooling to room temperature, washed product is collected product with magnet again, and oven dry obtains graphene-supported ferroferric oxide magnetic nanoparticle matrix material.
Graphite oxide in the described step (1) is commercially available; Or by following method preparation, the preparation method comprises:
Get Graphite Powder 99 and SODIUMNITRATE, stir after adding concentration afterwards and be the ice sulfuric acid of 98wt%, put into ice bath then, slowly add potassium permanganate when stirring, this moment, temperature remained at below 20 ℃, be warming up to 35 ± 5 ℃ and be incubated 1～2h then, reaction finishes the back and slowly adds deionized water, wherein the volume ratio of the deionized water of Jia Ruing and the vitriol oil is 2: 1, and temperature risen to 85～95 ℃, insulation 15min, add the 10ml massfraction again and be 30% hydrogen peroxide and deionized water, the deionized water that add this moment and the volume ratio of the vitriol oil are 6: 1, and products therefrom is through centrifugal, the 5wt%HCl washing, oven dry, grind, obtain the graphite oxide powder at last; Wherein the mass ratio of Graphite Powder 99 and SODIUMNITRATE is 2: 1, and the ratio of ice sulfuric acid and Graphite Powder 99 is 23ml/mg, and the mass ratio of potassium permanganate and Graphite Powder 99 is 3: 1.
The mass percent of hydrazine hydrate is 85% in the described step (1).
What described step (1) ultrasonic procedure adopted is that power is the ultrasonic processor of 300W, and ultrasonic time is 60～100min.
Described step (1) anion surfactant is sodium lauryl sulphate (SDS), Sodium dodecylbenzene sulfonate (SDBS), sodium polystyrene sulfonate (PSS) or polyacrylic acid (PAA), preferentially uses sodium lauryl sulphate (SDS).
Described step (2) trivalent iron salt and divalent iron salt comprise muriate, nitrate, nitrite, the vitriol of iron.Preferential iron chloride (the FeCl that uses
36H
2O, FeCl
24H
2O), Fe wherein
3+With Fe
2+Mol ratio be 2: 1.
The concentration of ammoniacal liquor is 6～10M in the described step (2), the pH=11 of solution～12.
The present invention is an initial feed with the graphite oxide of Hummers method preparation, with SDS modification is carried out on the surface of Graphene and is handled; Graphene after the modification is distributed in the aqueous solution, adds the molysite of trivalent and divalence again, adopt chemical precipitation method to prepare graphene-supported ferroferric oxide magnetic nanoparticle matrix material.
Beneficial effect
(1) the present invention adopts the anion surfactant modified graphene, has both improved the dispersiveness of Graphene in the aqueous solution, makes the Graphene surface with going up a large amount of negative charges again;
(2) ferroferric oxide magnetic nanoparticle by electrostatic adhesion on the Graphene surface;
(3) ferroferric oxide magnetic nanoparticle that loads on the Graphene is little, advantages of good crystallization, even particle distribution;
(4) preparation technology is simple, and production unit is required simply to be easy to suitability for industrialized production;
(5) prepared matrix material crystalline phase is pure, be evenly distributed, electrocatalysis is active good.
Description of drawings
The atomic power Scanning Probe Microscopy photo of Graphene after Fig. 1 .SDS modification;
Fig. 2. the X-ray diffractogram of graphene-supported ferroferric oxide magnetic nanoparticle matrix material;
Fig. 3. the transmission electron microscope photo of graphene-supported ferroferric oxide magnetic nanoparticle matrix material;
Fig. 4. the high-resolution-ration transmission electric-lens photo of graphene-supported ferroferric oxide magnetic nanoparticle matrix material;
Fig. 5. the cyclic voltammetry curve of graphene-supported ferroferric oxide magnetic nanoparticle matrix material.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Get Graphite Powder 99 and SODIUMNITRATE, stir after adding concentration afterwards and be the ice sulfuric acid of 98wt%, put into ice bath then, slowly add potassium permanganate when stirring, this moment, temperature remained at below 20 ℃, be warming up to 35 ± 5 ℃ and be incubated 1～2h then, reaction finishes the back and slowly adds deionized water, and temperature risen to 85～95 ℃, insulation 15min, add the 10ml massfraction again and be 30% hydrogen peroxide and deionized water, products therefrom through centrifugal, 5wt%HCl washing, oven dry, grind, obtain the graphite oxide powder at last; Wherein the mass ratio of Graphite Powder 99 and SODIUMNITRATE is 2: 1, the ratio of ice sulfuric acid and Graphite Powder 99 is 23ml/mg, the mass ratio of potassium permanganate and Graphite Powder 99 is 3: 1, and the volume ratio of the deionized water of Jia Ruing and the vitriol oil is 2: 1 first, and the deionized water that adds and the volume ratio of the vitriol oil are 6: 1 for the second time.
The graphite oxide that takes by weighing the above-mentioned preparation of 200mg adds in the beaker, add the 200ml deionized water again, ultra-sonic dispersion 60min, the unpeeled graphite flake of centrifugal then removal obtains the graphite oxide aqueous solution, solution is poured in the there-necked flask, adding 2ml massfraction is 85% hydrazine hydrate and 0.1gSDS, and magnetic agitation also is heated to 100 ℃, condensing reflux 20h.Graphene dispersion liquid oven dry with modification after reaction finishes adds water to 50ml again, and ultra-sonic dispersion is poured in the there-necked flask behind the macrobead in the centrifugal removal solution.Take by weighing high iron(ic) chloride of 0.2703g and 0.0994g four water iron protochlorides then in the 50ml deionized water, toward the logical nitrogen 10min of the aqueous solution, again with Fe
3+And Fe
2+The aqueous solution pour in the above-mentioned Graphene dispersion liquid, dropwise add the ammonia soln of 8M behind the ultrasonic agitation 10min, make mixing solutions pH=11～12.After question response finishes, again mixed solution is heated to 50 ℃ and keep 30min.Use the deionized water wash product to neutral after reacting completely repeatedly, and utilize magnet to collect product,, grind the matrix material that obtains graphene-supported ferroferric oxide magnetic nanoparticle at last with washing with alcohol and at 60 ℃ of following vacuum drying 24h.Fig. 1 is the atomic power Scanning Probe Microscopy photo of Graphene after the SDS modification, and as can be seen: the graphene film surface after the modification is also rough, has certain fold, and lamellar spacing reaches 2.525nm.Fig. 2 is the X-ray diffractogram of matrix material, and the diffraction peak among the figure shows: this nano composite material is Graphene-Z 250.Fig. 3 is the transmission electron microscope photo of matrix material, and as can be seen: ferroferric oxide nano granules covers on the Graphene lamella equably.Fig. 4 is the high-resolution-ration transmission electric-lens photo of matrix material, and as can be seen: the Z 250 that loads on the Graphene lamella is the irregular nano particle that size is about 10～30nm.Fig. 5 is the cyclic voltammetry curve of matrix material, and as can be seen: the redox electric current of composite electrode significantly improves, and has shown good electro catalytic activity.
Embodiment 2
Taking by weighing 220mg graphite oxide (commercially available) adds in the beaker, add the 220ml deionized water again, ultra-sonic dispersion 80min, the unpeeled graphite flake of centrifugal then removal obtains the graphite oxide aqueous solution, solution is poured in the there-necked flask, adding 2.2ml massfraction is 85% hydrazine hydrate and 0.11gSDBS, and magnetic agitation also is heated to 110 ℃, condensing reflux 22h.Graphene dispersion liquid oven dry with modification after reaction finishes adds water to 50ml again, and ultra-sonic dispersion is poured in the there-necked flask behind the macrobead in the centrifugal removal solution.Take by weighing high iron(ic) chloride of 0.3784g and 0.1391g four water iron protochlorides then in the 50ml deionized water, toward the logical nitrogen 20min of the aqueous solution, again with Fe
3+And Fe
2+The aqueous solution pour in the above-mentioned Graphene dispersion liquid, dropwise add the ammonia soln of 8M behind the ultrasonic agitation 10min, make mixing solutions pH=11～12.After question response finishes, again mixed solution is heated to 60 ℃ and keep 40min.Use the deionized water wash product to neutral after reacting completely repeatedly, and utilize magnet to collect product,, grind and obtain graphene-supported ferroferric oxide magnetic nanoparticle matrix material at last with washing with alcohol and at 60 ℃ of following vacuum drying 24h.The AFM photo is observed and shown: the graphene film after the modification is rough, has certain fold, and lamellar spacing reaches 2.525nm.The XRD test result shows: the synthetic matrix material is Graphene-Z 250.Transmission electron microscope observing shows: ferroferric oxide nano granules loads on the Graphene lamella equably.The high-resolution-ration transmission electric-lens photo is observed and shown: the Z 250 that loads on the Graphene lamella is the irregular nano particle that size is about 10～30nm.The cyclic voltammetry curve test shows: the redox electric current of composite electrode significantly improves, and has shown good electro catalytic activity.
Taking by weighing the previously prepared graphite oxide of 240mg adds in the beaker, add the 240ml deionized water again, ultra-sonic dispersion 100min, the unpeeled graphite flake of centrifugal then removal obtains the graphite oxide aqueous solution, solution is poured in the there-necked flask, adding 2.4ml massfraction is 85% hydrazine hydrate and 0.12gPSS, and magnetic agitation also is heated to 120 ℃, condensing reflux 24h.Graphene dispersion liquid oven dry with modification after reaction finishes adds water to 50ml again, and ultra-sonic dispersion is poured in the there-necked flask behind the macrobead in the centrifugal removal solution.Take by weighing high iron(ic) chloride of 0.4865g and 0.1789g four water iron protochlorides then in the 50ml deionized water, toward the logical nitrogen 30min of the aqueous solution, again with Fe
3+And Fe
2+The aqueous solution pour in the above-mentioned Graphene dispersion liquid, dropwise add the ammonia soln of 8M behind the ultrasonic agitation 10min, make mixing solutions pH=11～12.After question response finishes, again mixed solution is heated to 70 ℃ and keep 50min.Use the deionized water wash product to neutral after reacting completely repeatedly, and utilize magnet to collect product,, grind and obtain graphene-supported ferroferric oxide magnetic nanoparticle matrix material at last with washing with alcohol and at 60 ℃ of following vacuum drying 24h.The AFM photo is observed and shown: the graphene film after the modification is rough, has certain fold, and lamellar spacing reaches 2.525nm.The XRD test result shows: the synthetic matrix material is Graphene-Z 250.Transmission electron microscope observing shows: ferroferric oxide nano granules loads on the Graphene lamella equably.The high-resolution-ration transmission electric-lens photo is observed and shown: the Z 250 that loads on the Graphene lamella is the irregular nano particle that size is about 10～30nm.The cyclic voltammetry curve test shows: the redox electric current of composite electrode significantly improves, and has shown good electro catalytic activity.
Claims (7)
1. the preparation method of a graphene-supported ferroferric oxide magnetic nanoparticle matrix material comprises:
(1) taking by weighing 200～240mg graphite oxide is scattered in the deionized water of 200～240ml, ultrasonic 60～100min, pour in the container after centrifugal, container is put into oil bath pan, the anion surfactant that adds 2～3ml hydrazine hydrate and 0.1～0.2g, be heated to 100～120 ℃, condensing reflux 20～24 hours is cooled to the Graphene that oven dry after the room temperature obtains modification;
(2) Graphene that takes by weighing above-mentioned modification is scattered in the aqueous solution, and ultrasonic agitation is centrifugal, the Graphene dispersion liquid of modification; Take by weighing solubility trivalent iron salt and divalent iron salt, be dissolved in deionized water, feed nitrogen 10～30min, pour into then in the Graphene dispersion liquid of described modification, after ultrasonic agitation is even, dropping ammonia, after dripping end mixed solution is heated to 50～70 ℃, reaction 30～60min, question response finish postcooling to room temperature, washing, collection product, oven dry obtains graphene-supported ferroferric oxide magnetic nanoparticle matrix material.
2. the preparation method of a kind of graphene-supported ferroferric oxide magnetic nanoparticle matrix material according to claim 1 is characterized in that: the preparation method of the graphite oxide in the described step (1) comprises:
Get Graphite Powder 99 and SODIUMNITRATE, stir after adding concentration afterwards and be the ice sulfuric acid of 98wt%, put into ice bath then, slowly add potassium permanganate when stirring, this moment, temperature remained at below 20 ℃, be warming up to 35 ± 5 ℃ and be incubated 1～2h then, reaction finishes the back and slowly adds deionized water, and temperature risen to 85～95 ℃, insulation 15min, add the 10ml massfraction again and be 30% hydrogen peroxide and deionized water, products therefrom through centrifugal, 5wt%HCl washing, oven dry, grind, obtain the graphite oxide powder at last; Wherein the mass ratio of Graphite Powder 99 and SODIUMNITRATE is 2: 1, the ratio of ice sulfuric acid and Graphite Powder 99 is 23ml/mg, the mass ratio of potassium permanganate and Graphite Powder 99 is 3: 1, and the volume ratio of the deionized water of Jia Ruing and the vitriol oil is 2: 1 first, and the deionized water that adds and the volume ratio of the vitriol oil are 6: 1 for the second time.
3. the preparation method of a kind of graphene-supported ferroferric oxide magnetic nanoparticle matrix material according to claim 1 is characterized in that: the massfraction of hydrazine hydrate is 85% in the described step (1).
4. the preparation method of a kind of graphene-supported ferroferric oxide magnetic nanoparticle matrix material according to claim 1 is characterized in that: described step (1) anion surfactant is sodium lauryl sulphate SDS, Sodium dodecylbenzene sulfonate SDBS, sodium polystyrene sulfonate PSS or polyacrylic acid PAA.
5. the preparation method of a kind of graphene-supported ferroferric oxide magnetic nanoparticle matrix material according to claim 1, it is characterized in that: described step (2) trivalent iron salt and divalent iron salt are muriate, nitrate, nitrite or the vitriol of iron, and wherein the mol ratio of trivalent iron salt and divalent iron salt is 2: 1.
6. a kind of according to claim 1 or 5 preparation method of graphene-supported ferroferric oxide magnetic nanoparticle matrix material, it is characterized in that: described trivalent iron salt and divalent iron salt are iron chloride FeCl
36H
2O, FeCl
24H
2O.
7. the preparation method of a kind of graphene-supported ferroferric oxide magnetic nanoparticle matrix material according to claim 1 is characterized in that: the concentration of ammoniacal liquor is 6～10M in the described step (2), the pH=11 of solution～12.
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