CN102745675A - Preparation method of spinel-type magnetic MFe2O4/graphene composite material - Google Patents
Preparation method of spinel-type magnetic MFe2O4/graphene composite material Download PDFInfo
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- CN102745675A CN102745675A CN201210213651XA CN201210213651A CN102745675A CN 102745675 A CN102745675 A CN 102745675A CN 201210213651X A CN201210213651X A CN 201210213651XA CN 201210213651 A CN201210213651 A CN 201210213651A CN 102745675 A CN102745675 A CN 102745675A
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Abstract
The invention discloses a preparation method of a spinel-type magnetic MFe2O4/graphene composite material. The preparation method utilizes a water-soluble metal M<2+> salt and a Fe<3+> salt as precursors and graphite oxide as a matrix and comprises the following steps of carrying out ultrasonic dispersion of graphite oxide in ethanol or water as a solvent to obtain a graphene oxide dispersion, adding a M<2+> salt and Fe<3+> salt-containing aqueous solution having a M<2+>/Fe<3+> mole ratio of 1: 2 into the graphene oxide dispersion, fully stirring to obtain a mixed solution, adjusting a pH value of the mixed solution to a value more than 10 by an alkali liquor, adding a reducing agent into the mixed solution, stirring at a temperature of 80 to 150 DEG C for a reaction lasting for 4 to 10 hours, after the reaction is finished, carrying out separation, washing, drying and grinding, and carrying out calcination of the grinded powder at a temperature of 300 DEG C in a nitrogen or argon atmosphere for 2 to 10 hours. Magnetic MFe2O4 nano particles of the spinel-type magnetic MFe2O4/graphene composite material have high loading capacity, stable structures, good uniformity, good dispersibility and strong adhesion with graphene. The spinel-type magnetic MFe2O4/graphene composite material can be widely used in the fields of magnetic targeting materials and other related function materials.
Description
One, technical field
The present invention relates to grapheme material processing and applied technical field, specifically is spinel type magnetic MFe
2O
4The preparation method of/graphene composite material.
Two, background technology
Graphene is to pass through sp by carbon atom as one of member of charcoal family
2Hydridization, the cellular two-dimensional grid structure of the individual layer of formation.Graphene is the elementary cell that constitutes other carbon allotropes.2004, the physics professor Geim of Univ Manchester UK etc. peeled off the method for highly oriented pyrolytic graphite repeatedly with adhesive tape, have obtained the Graphene of stable existence.This discovery has caused physicist, chemist and material scholar's extensive concern immediately, has started the research boom again after soccerballene and carbon nanotube.As a kind of two dimensional crystal of uniqueness, Graphene has very excellent performance.Big like specific surface area, theoretical value is 2630m
2/ g; Superior, Young's modulus reaches 1.0TPa; Thermal conductivity is 5300Wm
-1K
-1, be more than 10 times of copper thermal conductivity; Almost completely transparent, light had only 2.3% absorption.The character that these are excellent makes Graphene in catalysis, important use will be arranged.In view of Graphene has regular two-dimensional surface structure, preparation is controlled, can be used as an ideal template supported catalyst, this is the ideal model system that provides of research load property catalyzer.Nano-metal-oxide/Graphene composite table reveals some special performances, and demonstrates many conventional solid specific performances that are different from, and has showed wide application prospect in fields such as environment, the energy, material, chemistry, pharmacy, military affairs.
Spinel type ferrite MFe
2O
4(M=Mn
2+, Zn
2+, and Ni
2+Deng) high as its operating frequency of a kind of magneticsubstance, the magnetic spectrum characteristic is good, has been widely used in aspects such as mutual inductance device, magnetic core bearing, transfer lever, information storage, magnetic fluid, microwave absorbing and medical diagnosis at present.The spinel type magneticsubstance is of a great variety.Different positively charged ions gets into spinel structure, has multiple combination of charge, for the investigator provides a huge experimental system.When particle size was nano level, each particle can be regarded a single magnetic domain as, and its multiple electromagnetic property or physical property promptly change and show superparamagnetism.In recent years; The preparation of magnetic Nano material more and more receives people's attention; Developing dissimilar nanometer ferrite matrix materials becomes the focus of current magneticsubstance research; Key is to seek how to utilize cheap raw material, takes simple but effective method to come processability excellent magnetism nano material.Employing hydrothermal methods such as the Wang Xin of Institutes Of Technology Of Nanjing have been synthesized magnetic MnFe
2O
4/ graphene composite catalyst be used to decompose methylene blue (Industrial&Engineering Chemistry Research, 2011.51 (2): 725-731), research shows, under the condition of visible light because MnFe
2O
4Cause composite catalyst to have very high activity with the interaction of Graphene.
Yet, at present based on magnetic MFe
2O
4The research of/graphene composite material is also just at the early-stage, prepared complex technical process and prepared MnFeO
4Be prone to characteristics such as reunion, therefore seek mutually pure, the difficult reunion of a kind of simple and easy preparation, the higher magnetic MFe of the specific magnetising moment
2O
4The method of/graphene composite material becomes the focus of research.Graphite itself is a kind of hydrophobic nature material, compares with it, and graphene oxide surface and edge have groups such as a large amount of hydroxyls, carboxyl, epoxy, and the existence of these polar groups makes graphite oxide in the aqueous solution, have good interlayer adsorptivity.Therefore, utilize the adsorbable a large amount of ionic characteristics of graphite oxide interlayer to make transition metal ion be adsorbed onto the graphite oxide interlayer, be reduced into transition metal oxide through certain mode again, the present invention adopts this method to prepare magnetic MFe
2O
4/ graphene composite material.Magnetic MFe
2O
4/ graphene composite material is as a kind of functional composite material that application potential is arranged very much, and in the preparation process, will solve following two problems: how (1) improves charge capacity; (2) how to improve MFe
2O
4And the bonding force between the Graphene.
Three, summary of the invention
The object of the present invention is to provide a kind of spinel type magnetic MFe
2O
4/ graphene composite material, technical problem to be solved are magnetic MFe
2O
4The preparation method that bonding force is strong between nanoparticle and the Graphene, charge capacity is high and technology is simple, with low cost, be applicable to suitability for industrialized production.
With water-soluble metal M
2+Salt and Fe
3+For presoma, with the graphite oxide is matrix; Comprise dispersion, mixing, reduction, separation, washing, drying, grinding and roasting, difference with the prior art is that described dispersion is that graphite oxide ultra-sonic dispersion in ethanol or water solvent obtains the graphene oxide dispersion liquid; Described mixing is with M
2+And Fe
3+The M of mol ratio 1:2
2+Salt and Fe
3+Fully mix in the salt brine solution adding graphene oxide dispersion liquid and obtain mixed solution; To be mixed solution o'clock add reductive agent in 80-150 ℃ of stirring reaction 4-10 hour with lye pH adjustment value＞10 in described reduction; Reaction finishes back separation, washing, drying and grinding and obtains powder, and described roasting is that powder obtained load spinel type MFe on Graphene in 300 ℃ of roasting 2-10 hours in inert atmosphere
2O
4The title product spinel type magnetic MFe of nano particle
2O
4/ graphene composite material.
The concrete operations step is following:
A, graphite oxide is added in ethanol or the water equal solvent, ultra-sonic dispersion 30-60min obtains the graphene oxide dispersion liquid of homogeneous;
B, with M
2+And Fe
3+The metal M of mol ratio 1:2
2+Salt and Fe
3+Salt is soluble in water, joins in the graphene oxide dispersion liquid, fully mixes and obtains mixed solution;
C, transfer the pH of mixed value with alkali lye>10, add an amount of reductive agent down constantly stirring, fully react 4-10h down at 80-150 ℃;
D, product adopt centrifugal or magnetic separates, and successively with zero(ppm) water or absolute ethanol washing, drying is ground;
Sample roasting 2-10h under inert atmosphere after e, the grinding obtains MFe
2O
4/ graphene composite material.
Described water-soluble metal M
2+The M of salt
2+Be selected from Mn
2+, Zn
2+, or Ni
2+In a kind of.
Described reductive agent is selected from Hydrazine Hydrate 80 and Peng Qinghuana.
Described alkali lye is selected from a kind of in NaOH solution, KOH solution or the ammoniacal liquor.
Described inert atmosphere is selected from nitrogen or argon gas.
Utilize the spinel type magnetic MFe of the inventive method preparation
2O
4/ graphene composite material, its electronic scanning electron microscope (SEM) and transmission electron microscope (TEM) show, have deposited MFe more equably on the Graphene surface
2O
4Particle, its median size about 30nm, MFe
2O
4Nanoparticle and Graphene have stronger bonding force, in ultra-sonic dispersion and high-speed stirring process, can not break away from Graphene.Its X-ray diffraction curve (XRD) shows, the graphene-supported magnetic MFe of preparation
2O
4The purity of particle is higher.
Compared with present technology, beneficial effect of the present invention is embodied in:
Gained spinel type magnetic MFe of the present invention
2O
4Magnetic MFe in the/graphene composite material
2O
4Nanometer particle load amount height, Stability Analysis of Structures, evenly, good dispersivity, and and Graphene between stronger bonding force is arranged.Preparation technology of the present invention has efficiently, environmental protection, advantage of simple technology, this spinel type magnetic MFe
2O
4/ graphene composite material can be widely used in magnetic target material, various catalyzer, aspect and other relevant field of functional materials such as electromagnetic shielding absorbing material, electrode material for super capacitor.
Four, description of drawings
Figure l is the spinel type magnetic MnFe of embodiment 1 preparation
2O
4/ graphene composite material SEM (a) and TEM (b) photo, and XRD figure (c);
Fig. 2 is the spinel type magnetic ZnFe of embodiment 2 preparations
2O
4/ graphene composite material SEM (a) and TEM (b) photo, and XRD figure (c);
Five, embodiment
Below pass through the specific embodiment, and in conjunction with the accompanying drawings the present invention is further described.
Embodiment 1:
Spinel type magnetic MFe
2O
4The preparation technology of/graphene composite material (M=Mn), operating process is following:
The first step: in the 300mL distilled water solution that the graphite oxide of 0.9g is joined, ultra-sonic dispersion 30min obtains the graphene oxide dispersion liquid of homogeneous;
Second step: the Mn (CH of 0.52g
3COO)
24H
2O and 1.72g Fe (NO)
39H
2O is dissolved in (Mn in the 25mL water
2+And Fe
2+Mol ratio be 1:2), join in the graphene oxide dispersion liquid, fully mix and obtain mixed solution;
The 3rd step: use content is 10% sodium hydroxide solution accent pH of mixed value>10, the content that under constantly stirring, adds 15mL is 50% Hydrazine Hydrate 80, the abundant 4h that reacts under 80-150 ℃ of constant temperature;
The 4th step: product adopts centrifugal or magnetic separates, and successively with zero(ppm) water or absolute ethanol washing, drying is ground;
The 4th step: the sample after the grinding is 300 ℃ of following roasting 3h under nitrogen atmosphere, obtain spinel type magnetic MnFe
2O
4/ graphene composite material.
Embodiment 2:
Different is with embodiment 1, in the present embodiment, in step 2, with the Mn (CH of 0.52g
3COO)
24H
2O replaces with the Zn (CH of 0.467g
3COO)
22H
2O, operation steps and other requirement are all identical with embodiment 1.Through behind the purifying, obtain spinel type magnetic ZnFe
2O
4/ graphene composite material.
Embodiment 3:
Different is with embodiment 1, in the present embodiment, in step 2, with the Mn (CH of 0.52g
3COO)
24H
2O replaces with the Ni (NO of 0.617g
3)
26H
2O, operation steps and other requirement are all identical with embodiment 1.Through behind the purifying, obtain spinel type magnetic NiFe
2O
4/ graphene composite material.
Embodiment 4:
Different is with embodiment 1, in the present embodiment, in step 3, is 50% Hydrazine Hydrate 80 with the content of 15mL, and the Peng Qinghuana, operation steps and other requirement that replace with 15mg are all identical with embodiment 1.Through behind the purifying, obtain spinel type magnetic MnFe
2O
4/ graphene composite material.
Embodiment 5:
Different is with embodiment 1, and in the present embodiment, in step 3, using content is 10% sodium hydroxide solution, and it is all identical with embodiment 1 to replace with content and be 28% ammonia soln, operation steps and other requirement.Through behind the purifying, obtain spinel type magnetic MnFe
2O
4/ graphene composite material.
Claims (4)
1. spinel type magnetic MFe
2O
4The preparation method of/graphene composite material is with water-soluble metal M
2+Salt and Fe
3+For presoma, with the graphite oxide is matrix, comprises dispersion, mixing, reduction, separation, washing, drying, grinding and roasting, it is characterized in that: described dispersion is that graphite oxide ultra-sonic dispersion in ethanol or water solvent obtains the graphene oxide dispersion liquid; Described mixing is with M
2+And Fe
3+The M of mol ratio 1:2
2+Salt and Fe
3+Fully mix in the salt brine solution adding graphene oxide dispersion liquid and obtain mixed solution; To be mixed solution o'clock add reductive agent in 80-150 ℃ of stirring reaction 4-10 hour with lye pH adjustment value＞10 in described reduction; Reaction end back separation, washing, dry and grinding; Described roasting be with the powder after grinding in nitrogen or argon gas atmosphere in 300 ℃ of roasting 2-10 hours.
2. spinel type magnetic MFe according to claim 1
2O
4The preparation method of/graphene composite material is characterized in that: described water-soluble metal M
2+The M of salt
2+Be selected from Mn
2+, Zn
2+, or Ni
2+In a kind of.
3. spinel type magnetic MFe according to claim 1
2O
4The preparation method of/graphene composite material is characterized in that: described reductive agent is selected from Hydrazine Hydrate 80 or Peng Qinghuana.
4. spinel type magnetic MFe according to claim 1 and 2
2O
4The preparation method of/graphene composite material is characterized in that: described alkali lye is selected from a kind of in NaOH solution, KOH solution or the ammoniacal liquor.
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