CN102660220A - Preparation method of graphene supported ferriferrous oxide nanocomposite - Google Patents
Preparation method of graphene supported ferriferrous oxide nanocomposite Download PDFInfo
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- CN102660220A CN102660220A CN2012101096731A CN201210109673A CN102660220A CN 102660220 A CN102660220 A CN 102660220A CN 2012101096731 A CN2012101096731 A CN 2012101096731A CN 201210109673 A CN201210109673 A CN 201210109673A CN 102660220 A CN102660220 A CN 102660220A
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Abstract
The invention discloses a preparation method of a graphene supported ferriferrous oxide nanocomposite, comprising the following steps: preparing a precursor by deposition precipitation method, depositing ferric nitrate ninehydrate or ferric chloride hexahydrate on graphene in the form of iron hydroxide by using sodium hydroxide or ammonia to obtain black powder, washing and drying the obtained black powder, grinding the dried black powder, then calcining under the protection of argon, and then cooling, and reducing under the protection of a mixed gas of argon and hydrogen or argon and ammonia gas to obtain the graphene supported ferriferrous oxide nanocomposite. The preparation method is simple and stable. In the obtained composite, ferriferrous oxide is uniformly distributed on graphene and has good interface combination of the substrate graphene, thus the absorbing properties and the like of the composite as a functional material can be improved. The method also can be used for preparing carbon material supported ferriferrous oxide nanocomposites with different substrates by using carbon nanotube, graphite oxide and other carbon materials as the substrate.
Description
Technical field
The present invention relates to a kind of preparation method of graphene-supported ferriferrous oxide nano matrix material, belong to the technical field of nano composite material.
Background technology
Graphene is a kind of novel two-dimentional carbon nanomaterial that utilized the method for the high oriented graphite of tape stripping to obtain by the Novoslov of Univ Manchester UK etc. in 2004, and is tightly packed by carbon atom, can be regarded as " graphite flake " that one deck is stripped from.Graphene has excellent physical chemistry, since coming to light from it with its matrix material that obtains as matrix load oxide compound just by extensive concern.Domestic and international research personnel have carried out extensive studies to the preparation of graphene-supported ferriferrous oxide composite material; Because Graphene good electrical properties; And the magnetic property of Z 250; Their matrix material can be applied to magnetic resonance contrast agent, lithium ion battery, energy storage and fields such as release and absorption of electromagnetic wave, and the realization of these application all be unable to do without the good electrical properties or the magnetic property of graphene-supported ferriferrous oxide composite material, and the combination of electrical property and magnetic property; In order to improve its performance as functional materials, the researchist adopts various preparing methods in the hope of obtaining the matrix material of better performance.
The preparation method of the graphene-supported ferriferrous oxide composite material of preparation mainly comprises following two kinds at present:
(1) solvent-thermal method: be about to Z 250 and Graphene, and in reaction compound stirring and dissolving in reductive agent such as acting sodium acetate, mixing solutions is put in the teflon-lined reaction kettle method of at high temperature reacting.This method is to prepare a kind of method that derives on the method basis of Z 250 at solvent-thermal method, and this method technology is simple, but parameter is too much; Like temperature, the add-on of time and raw material, the amount of reductive agent etc.; Wayward, and the magnetic property of its gained matrix material a little less than, be not easy to application as absorbing material; And the Graphene preparation adopts oxide-reduction method to obtain mostly; The most crystallization degree of the grapheme material that obtains is poor, and therefore the sheet bed thickness also hinders its application as battery material.
(2) coprecipitation method: promptly under nitrogen atmosphere, divalent iron salt, trivalent iron salt are mixed stirring at a certain temperature with Graphene, synthesize the method for Z 250 afterwards through the sodium hydroxide titration.This method mainly is that to be main raw material through the method that in basic soln, combines to prepare Z 250 derive obtains with ferrous iron and ferric iron; The ferriferrous oxide particles that this method obtains is less; And because particle is not done modification; Thereby be difficult for combining to be difficult to successful load with grapheme material, even in the load, the very difficult uniform loading because the big characteristics of its small-particle surface energy are very easily reunited.These all can influence the application of matrix material as functional materials.
People [Feng Jiao, Jean-Claude Jumas, et al. Synthesis of Ordered Mesoporous Fe such as Feng Jiao
3O
4And γ-Fe
2O
3With Crystalline Walls Using Post-Template Reduction/Oxidation [J]. Journal of the American Chemical Society. 2006,128 (39): 12905-12909.] method through first reduction rear oxidation is α-Fe
2O
3Be reduced into Fe
3O
4, oxidation obtains γ-Fe in air again
2O
3No matter hence one can see that is α-Fe
2O
3Or γ-Fe
2O
3Can obtain Fe through the effect of reducing atmosphere
3O
4
" CN201110207639.3 " patent has proposed to obtain with annealing the matrix material of graphene-supported Z 250, and its method mainly is with Graphene and Fe (NO)
39H
2O is soluble in water, through the centrifugal throw out that obtains, after ethanol and washed with de-ionized water; At 350 ℃ of 2h that anneal down, thereby obtain graphene-supported ferriferrous oxide composite material, this method uses simple method for calcinating to replace above two kinds of methods; Reduced the difficulty of operation; And reduced the parameter of reaction, made and react more stable and controllable, still; The weak point of this method is: 1. because the raw material molysite all is water-soluble, therefore in centrifugal process, cause a large amount of losses of iron ion unavoidably; 2. in calcination process, do not have reducing atmosphere, be difficult to the molysite calcining and decomposing is become Z 250.
To sum up; Adopt simple and stable synthesis technique; Preparing ferroferric oxide nano granules can homodisperse; And loading on the Graphene surface in a large number is the key of the graphene-supported ferriferrous oxide composite material of preparation, and this is also for further the excellent electrical or the magnetic property of performance matrix material lay the first stone.
Summary of the invention
The object of the invention is to provide a kind of preparation method of graphene-supported ferriferrous oxide nano matrix material, and this method advantage is the technology simple and stable, and the matrix material that makes has good performance.
The present invention realizes that through following technical scheme a kind of preparation method of graphene-supported ferriferrous oxide nano matrix material is characterized in that comprising following process:
1) deposition-precipitation method prepares presoma
With Graphene and Fe (NO)
39H
2O or and FeCl
36H
2O presses mass ratio 1:0.2 ~ 1 and adds in the absolute ethyl alcohol, obtains mixed solution A, uses the X 2073 of 200mg or the consumption of sodium lauryl sulphate by every gram Graphene; In the mixed solution A of Graphene and source of iron, add X 2073 or sodium lauryl sulphate; Ultrasonic 5 ~ 10min in ultrasonator stirs 1 ~ 2h down for 30 ~ 80 ℃ in temperature then, obtains mixing solutions B; In whipping process, according to every gram Fe (NO)
39H
2O uses the NaOH of 279mg or according to every gram FeCl
36H
2O uses the consumption of the NaOH of 444mg, or according to every gram Fe (NO)
39H
2The O working concentration is the ammoniacal liquor 0.289mL of 0.9g/mL or according to every gram FeCl
36H
2The O working concentration is the ammoniacal liquor 0.432mL of 0.9g/mL; With the ammoniacal liquor after NaOH solution or the dilution with 10-30 drip/min splashes among the gained mixing solutions B; Dropwise back restir 0.5 ~ 1.5h; Using deionized water that resulting black powder is washed till pH then is 7, at 60 ~ 100 ℃ of oven dry of temperature 8-12h, obtains Fe (OH)
3/ Graphene precursor powder;
2) calcining and decomposing of presoma and reduction
(1) the resulting precursor powder of step 1) is spread out and put in quartz boat; Quartz boat places the tube furnace flat-temperature zone; Flow with 100-300mL/min feeds the 5-30min argon gas to drain air; Temperature rise rate with 7.5 ~ 10 ℃/min is warming up to 400 ~ 600 ℃, calcining at constant temperature 0.5 ~ 3h under argon shield afterwards;
(2) the calcining continued feeds argon gas; The tube furnace temperature is cooled to 200 ~ 400 ℃ with the rate of temperature fall of 7.5 ~ 10 ℃/min, reduce argon flow amount, and feed hydrogen or ammonia to 80-120mL/min; Reduce with argon gas and hydrogen or with the mixed gas of argon gas and ammonia; The volume flow ratio of argon gas and hydrogen or argon gas and ammonia is (0.85 ~ 0.95): (0.05 ~ 0.15), reduction 30 ~ 90min obtains graphene-supported ferriferrous oxide nano matrix material.
The present invention has the following advantages: preparation technology's simple and stable, and resultant matrix material, the Z 250 on the Graphene is evenly distributed; And combine well with matrix graphite alkene interface; Graphene-structured is good, and crystallization degree is better, can improve its performance such as suction ripple as functional materials.This method can promote also that to be used for carbon materials such as carbon nanotube, graphite oxides be the matrix material that matrix prepares the carbon material supported Z 250 of different matrix.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the employed Graphene of various embodiments of the present invention.
Fig. 2 makes the transmission electron microscope photo of graphene-supported Z 250 composite powder for the embodiment of the invention 1.
Fig. 3 makes the X ray diffracting spectrum of graphene-supported Z 250 composite powder for the embodiment of the invention 1.
Fig. 4 makes the magnetic hysteresis loop figure of graphene-supported Z 250 composite powder for the embodiment of the invention 1.
Embodiment
Further the present invention will be described below in conjunction with embodiment, and these embodiment only are used to explain the present invention, do not limit the present invention.
Embodiment 1
With the Graphene of 0.05g and the Fe of 0.05g (NO)
39H
2O adds in the 40mL absolute ethyl alcohol, stirs 1h at 60 ℃ of lower magnetic forces of temperature, and the X 2073 of weighing 0.004g adds in the above-mentioned solution, at room temperature continues afterwards to stir.Take by weighing the NaOH of 0.0149g, be dissolved in the 30mL water, after the dissolving, pour in the separating funnel, splash in the above-mentioned solution, after titration finishes, continue to stir 1h with the speed of 15/min.Filter with B then, the gained black powder use washed with de-ionized water to pH be 7, in 60 ℃ of baking ovens that temperature is, dry 12h.Powder after the oven dry is ground, and the gained powder is spread out and put in quartz boat, and quartz boat is placed the tube furnace flat-temperature zone; Flow with 200mL/min feeds the 10min argon gas to drain air, and the temperature rise rate with 7.5 ℃/min is warming up to 450 ℃ under argon shield afterwards, at this temperature calcining at constant temperature 2h; Afterwards with the speed of 10 ℃/min with tube furnace greenhouse cooling to 350 ℃; Argon flow amount is reduced to 95mL/min, and feed hydrogen, reduce with argon gas/hydrogen gas mixture with the flow of 5mL/min; Reduction 30min obtains graphene-supported ferriferrous oxide nano matrix material.
Embodiment 2
With the Graphene of 0.05g and the FeCl of 0.05g
36H
2O adds in the 60mL absolute ethyl alcohol, and the X 2073 of weighing 0.006g adds in the above-mentioned solution, stirs 1h at 60 ℃ of lower magnetic forces of temperature, at room temperature continues afterwards to stir.Take by weighing the NaOH of 0.0222g, be dissolved in the 30mL water, after the dissolving, pour in the separating funnel, splash in the above-mentioned solution, after titration finishes, continue to stir 1h with the speed of 15/min.Filter with B then, the gained black powder use washed with de-ionized water to pH be 7, be to dry 12h in 60 ℃ of baking ovens in temperature.Powder after the oven dry is ground, and the gained powder is spread out and put in quartz boat, and quartz boat is placed the tube furnace flat-temperature zone; Flow with 200mL/min feeds the 10min argon gas to drain air, and the temperature rise rate with 7.5 ℃/min is warming up to 450 ℃ under argon shield afterwards, at this temperature calcining at constant temperature 2h; Afterwards the tube furnace temperature is cooled to 350 ℃ with the rate of temperature fall of 10 ℃/min; Argon flow amount is reduced to 95mL/min, and feed hydrogen, reduce with argon gas/hydrogen gas mixture with the flow of 5mL/min; Reduction 30min obtains graphene-supported ferriferrous oxide nano matrix material.
Embodiment 3
With the Graphene of 0.02g and the Fe of 0.01g (NO)
39H
2O adds in the 40mL absolute ethyl alcohol, stirs 1h at 60 ℃ of lower magnetic forces of temperature, and the X 2073 of weighing 0.004g adds in the above-mentioned solution, at room temperature continues afterwards to stir.Take by weighing the NaOH of 0.003g, be dissolved in the 10mL water, after the dissolving, pour in the separating funnel, splash in the above-mentioned solution, after titration finishes, continue to stir 0.5h with the speed of 15/min.Filter with B then, the gained black powder use washed with de-ionized water to pH be 7, in temperature is 80 ℃ baking oven, dry 12h.Powder after the oven dry is ground, and the gained powder is spread out and put in quartz boat, and quartz boat is placed the tube furnace flat-temperature zone; Flow with 150mL/min feeds the 15min argon gas to drain air; Temperature rise rate with 7.5 ℃/min is warming up to 450 ℃ under argon shield afterwards, at this temperature calcining at constant temperature 1.5h, afterwards with the rate of temperature fall of 10 ℃/min with tube furnace greenhouse cooling to 400 ℃; Argon flow amount is reduced to 90mL/min; And feed hydrogen with the flow of 10mL/min, with argon gas/hydrogen gas mixture reduction 30min, obtain graphene-supported ferriferrous oxide nano matrix material.
Embodiment 4
With 0.02g Graphene and 0.01gFeCl
36H
2O adds in the 40mL absolute ethyl alcohol, stirs 1h at 60 ℃ of lower magnetic forces, and weighing 0.004g X 2073 adds in the above-mentioned solution, at room temperature continues afterwards to stir.Take by weighing 0.0045gNaOH, be dissolved in the 10mL water, after the dissolving, pour in the separating funnel, splash in the above-mentioned solution, after titration finishes, continue to stir 0.5h with the speed of 15/min.Filter with B then, the gained black powder use washed with de-ionized water to pH be 7, in 80 ℃ of baking ovens, dry 12h.Powder after the oven dry is ground, and the gained powder is spread out and put in quartz boat, and quartz boat is placed the tube furnace flat-temperature zone; Flow with 150mL/min feeds the 15min argon gas to drain air, and the temperature rise rate with 7.5 ℃/min is warming up to 400 ℃ under argon shield afterwards, and at this temperature calcining at constant temperature 1.5h; With the rate of temperature fall of 10 ℃/min the tube furnace temperature is reduced to 300 ℃ afterwards; Argon flow amount is reduced to 90mL/min, and feeds hydrogen with the flow of 10mL/min, reduces with argon gas/hydrogen gas mixture; Reduction 30min obtains graphene-supported ferriferrous oxide nano matrix material.
Embodiment 5
With the Graphene of 0.05g and the FeCl of 0.02g
36H
2O adds in the 80mL absolute ethyl alcohol, stirs 1.5h at 80 ℃ of lower magnetic forces of temperature, and the sodium lauryl sulphate of weighing 0.008g adds in the above-mentioned solution, at room temperature continues afterwards to stir.Measure 1mL ammoniacal liquor, be diluted in the 10mL deionized water, and pour in the separating funnel, splash in the above-mentioned solution, after titration finishes, continue to stir 1.5h with the speed of 15/min.Filter with B then, the gained black powder use washed with de-ionized water to pH be 7, be to dry 12h in 80 ℃ of baking ovens in temperature.Powder after the oven dry is ground, and the gained powder is spread out and put in quartz boat, and quartz boat is placed the tube furnace flat-temperature zone; Flow with 250mL/min feeds the 5min argon gas to drain air, and the temperature rise rate with 7.5 ℃/min is warming up to 500 ℃ under argon shield afterwards, and at this temperature calcining at constant temperature 2.5h; Afterwards the tube furnace temperature is cooled to 350 ℃ with the rate of temperature fall of 10 ℃/min; Argon flow amount is reduced to 85mL/min, and feeds hydrogen with the flow of 15mL/min, reduces with argon gas/hydrogen gas mixture; Reduction 45min obtains graphene-supported ferriferrous oxide nano matrix material.
Embodiment 6
With the Graphene of 0.05g and the Fe of 0.02g (NO)
39H
2O adds in the 80mL absolute ethyl alcohol, stirs 1.5h at 80 ℃ of lower magnetic forces, and the sodium lauryl sulphate of weighing 0.008g adds in the above-mentioned solution, at room temperature continues afterwards to stir.Take by weighing the NaOH of 0.006g, be dissolved in the 15mL water, after the dissolving, pour in the separating funnel, splash in the above-mentioned solution, after titration finishes, continue to stir 1.5h with the speed of 15/min.Filter with B then, the gained black powder use washed with de-ionized water to pH be 7, in 80 ℃ of baking ovens of temperature, dry 12h.Powder after the oven dry is ground, and the gained powder is spread out and put in quartz boat, and quartz boat is placed the tube furnace flat-temperature zone; Flow with 250mL/min feeds the 15min argon gas to drain air, and the temperature rise rate with 8 ℃/min is warming up to 500 ℃ under argon shield afterwards, and at this temperature calcining 2.5h; Afterwards the tube furnace temperature is reduced to 350 ℃ with the rate of temperature fall of 10 ℃/min; Argon flow amount is reduced to 85mL/min, and feeds hydrogen with the flow of 15mL/min, reduces with argon gas/hydrogen gas mixture; Reduction 45min obtains the graphene-supported ferriferrous oxide nano matrix material of graphene-supported ferriferrous oxide nano.
Embodiment 7
With the Graphene of 0.05g and the Fe of 0.02g (NO)
39H
2O adds in the 80mL absolute ethyl alcohol, stirs 1.5h at 80 ℃ of lower magnetic forces, and the sodium lauryl sulphate of weighing 0.008g adds in the above-mentioned solution, at room temperature continues afterwards to stir.Take by weighing the NaOH of 0.006g, be dissolved in the 15mL water, after the dissolving, pour in the separating funnel, splash in the above-mentioned solution, after titration finishes, continue to stir 1.5h with the speed of 15/min.Filter with B then, the gained black powder use washed with de-ionized water to pH be 7, in 80 ℃ of baking ovens of temperature, dry 12h.Powder after the oven dry is ground, and the gained powder is spread out and put in quartz boat, and quartz boat is placed the tube furnace flat-temperature zone; Flow with 250mL/min feeds the 15min argon gas to drain air, and the temperature rise rate with 7.5 ℃/min is warming up to 500 ℃ under argon shield afterwards, and at this temperature calcining 2.5h; Afterwards the tube furnace temperature is reduced to 350 ℃ with the rate of temperature fall of 8 ℃/min; Argon flow amount is reduced to 85mL/min, and feeds ammonia with the flow of 15mL/min, reduces with argon gas/ammonia gas mixture body; Reduction 60min obtains graphene-supported ferriferrous oxide nano matrix material.
Claims (1)
1. the preparation method of a graphene-supported ferriferrous oxide nano matrix material is characterized in that comprising following process:
1) deposition-precipitation method prepares presoma
With Graphene and Fe (NO)
39H
2O or and FeCl
36H
2O presses mass ratio 1:0.2 ~ 1 and adds in the absolute ethyl alcohol, obtains mixed solution A, uses the X 2073 of 200mg or the consumption of sodium lauryl sulphate by every gram Graphene; In the mixed solution A of Graphene and source of iron, add X 2073 or sodium lauryl sulphate; Ultrasonic 5 ~ 10min in ultrasonator stirs 1 ~ 2h down for 30 ~ 80 ℃ in temperature then, obtains mixing solutions B; In whipping process, according to every gram Fe (NO)
39H
2O uses the NaOH of 279mg or according to every gram FeCl
36H
2O uses the consumption of the NaOH of 444mg, or according to every gram Fe (NO)
39H
2The O working concentration is the ammoniacal liquor 0.289mL of 0.9g/mL or according to every gram FeCl
36H
2The O working concentration is the ammoniacal liquor 0.432mL of 0.9g/mL; With the ammoniacal liquor after NaOH solution or the dilution with 10-30 drip/min splashes among the gained mixing solutions B; Dropwise back restir 0.5 ~ 1.5h; Using deionized water that resulting black powder is washed till pH then is 7, at 60 ~ 100 ℃ of oven dry of temperature 8-12h, obtains Fe (OH)
3/ Graphene precursor powder;
2) calcining and decomposing of presoma and reduction
(1) the resulting precursor powder of step 1) is spread out and put in quartz boat; Quartz boat places the tube furnace flat-temperature zone; Flow with 100-300mL/min feeds the 5-30min argon gas to drain air; Temperature rise rate with 7.5 ~ 10 ℃/min is warming up to 400 ~ 600 ℃, calcining at constant temperature 0.5 ~ 3h under argon shield afterwards;
(2) the calcining continued feeds argon gas; The tube furnace temperature is cooled to 200 ~ 400 ℃ with the rate of temperature fall of 7.5 ~ 10 ℃/min, reduce argon flow amount, and feed hydrogen or ammonia to 80-120mL/min; Reduce with argon gas and hydrogen or with the mixed gas of argon gas and ammonia; The volume flow ratio of argon gas and hydrogen or argon gas and ammonia is (0.85 ~ 0.95): (0.05 ~ 0.15), reduction 30 ~ 90min obtains graphene-supported ferriferrous oxide nano matrix material.
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