CN104607228A - Preparation method for alpha-Fe2O3 quantum dot/nitrogen-doped graphene composite material - Google Patents
Preparation method for alpha-Fe2O3 quantum dot/nitrogen-doped graphene composite material Download PDFInfo
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- CN104607228A CN104607228A CN201510036230.8A CN201510036230A CN104607228A CN 104607228 A CN104607228 A CN 104607228A CN 201510036230 A CN201510036230 A CN 201510036230A CN 104607228 A CN104607228 A CN 104607228A
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Abstract
The invention discloses a preparation method for an alpha-Fe2O3 quantum dot/nitrogen-doped graphene composite material, relates to preparation methods for alpha-Fe2O3/graphene composite materials, and aims to solve a problem that ultra-dispersion characteristics of alpha-Fe2O3 quantum dots cannot be guaranteed while the alpha-Fe2O3 quantum dots grow on nitrogen-doped graphene in situ. The method comprises the following steps: 1, adding an alkali source and an inorganic iron solution into an organic matter aqueous solution containing hydroxyl groups; 2, adding graphene oxide into mixed liquor in the step 1, performing ultrasonic treatment, and stirring; 3, pouring suspension liquor obtained in the step 2 into a hydrothermal reaction kettle for reaction, cooling, performing centrifuging, washing, and drying. The method has the advantages that the average particle size of the alpha-Fe2O3 quantum dots in the composite functional material is small; a reaction condition is mild, equipment is simple, a reagent is low in price, safe and nontoxic, and large-scale production is facilitated; the photo-Fenton activity of the composite material is higher than that of commercial Fe2O3.
Description
Technical field
The present invention relates to a kind of α-Fe
2o
3the preparation method of/graphene composite material.
Background technology
Graphene, as a kind of novel two-dimension nano materials, because of the monoatomic layer crystal structure of its uniqueness, and has physico-chemical property (the such as high carrier mobility speed: 2 × 10 of many excellences
5cmV
-1s
-1), the specific area (2630m of superelevation
2g
-1) etc., and cause the extensive concern in the fields such as physics, chemistry, material.In recent years, round α-Fe
2o
3the preparation of/Graphene composite functional material, researcher expands large quantifier elimination, successfully prepares many α-Fe
2o
3/ graphene composite material, and be widely used in the numerous areas such as photocatalytic water, lithium ion battery, light degradation organic pollution.But still there is following problem in above-mentioned preparation method: α-Fe in (1) prepared composite
2o
3and non-homogeneous dispersion, reunite comparatively serious; (2) α-Fe in prepared composite
2o
3nanoscale still too large, be unfavorable for the carrying out of interfacial chemical reaction.Researcher finds, introduces heteroatom (such as nitrogen, phosphorus, boron etc.), can not only improve the photoelectrochemical behaviour of Graphene further, can also strengthen α-Fe in the lattice of Graphene
2o
3with the synergy of Graphene.Therefore, fall apart oversubscription α-Fe
2o
3quantum dot is organically combined with nitrogen-doped graphene, greatly will improve the physical and chemical performance of composite.But how to allow α-Fe
2o
3quantum dot growth in situ while nitrogen-doped graphene, and guarantees that the characteristic that its oversubscription is loose is problem demanding prompt solution.
Summary of the invention
The present invention cannot allow α-Fe at present in order to solve
2o
3quantum dot growth in situ guarantees α-Fe while nitrogen-doped graphene
2o
3the technical problem of the characteristic that quantum dot oversubscription is fallen apart, and a kind of α-Fe is provided
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite.
A kind of α-Fe of the present invention
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite carries out according to the following steps:
One, join in deionized water by the organic matter containing hydroxyl, mix and blend 5min ~ 10min, obtains organic solution; The aqueous solution of alkali source and inorganic iron is joined in organic solution successively, stirs 5min ~ 10min, form uniform transparent mixed liquor; Described is 1g:(0.5mL ~ 1mL containing the organic quality of hydroxyl and the volume ratio of deionized water); Described alkali source is 1:(100 ~ 200 with the organic mass ratio containing hydroxyl); The concentration of the aqueous solution of described inorganic iron is 0.05mol/L ~ 0.5mol/L; The volume of the aqueous solution of described inorganic iron is 1mL:(4.29g ~ 8.57g with the organic mass ratio containing hydroxyl);
Two, joined by graphene oxide in the uniform transparent mixed liquor that step one obtains, ultrasonic 0.3h ~ 2.0h, then stirs 2.0h ~ 4.0h, obtains stable suspension; Described graphene oxide and the organic mass ratio containing hydroxyl described in step one are 1:(750 ~ 1500);
Three, after stable suspension step 2 obtained pours hydrothermal reaction kettle into, be react 5h ~ 36h under the condition of 100 DEG C ~ 200 DEG C in temperature, naturally cool to room temperature, carry out centrifugal, then spend deionized water 3 times, 2 times are washed again with ethanol, finally dry 12h under temperature is the condition of 50 DEG C, obtains α-Fe
2o
3quantum dot/nitrogen-doped graphene composite.
Graphene oxide in step 2 of the present invention is standby by traditional Hummers legal system.
Principle of the present invention:
In the present invention, iron ion is due to electrostatic interaction, can be adsorbed on the graphenic surface of N doping, nucleating growth; In addition, because the organic matter containing hydroxyl contains multiple hydroxyl, it can effectively be adsorbed on α-Fe
2o
3nanocrystalline surface, therefore, the present invention adds a large amount of organic matters containing hydroxyl and makes α-Fe in preparation process
2o
3nanocrystalline surface is covered by the organic matter containing hydroxyl completely, to limit α-Fe
2o
3nanocrystalline further growth; Meanwhile, α-Fe is covered
2o
3nanocrystal surface containing the organic matter of hydroxyl can also effectively hinder nanocrystalline between reunion, and then obtain hyperfine α-Fe
2o
3quantum dot (mean size is 3.2nm), surpasses and is scattered on nitrogen-doped graphene sheet;
In composite prepared by the present invention, α-Fe
2o
3the average grain diameter of quantum dot is 3.2nm, and within the diffusion path scope of photohole, therefore photohole can effectively arrive α-Fe
2o
3the surface of quantum dot, and then oxidative degradation rhodamine B; Due to α-Fe
2o
3quantum dot is very little, and therefore its chemism point position exposed is more, therefore can effective rhodamine B degradation; Due to α-Fe
2o
3quantum dot be growth in situ on nitrogen-doped graphene sheet, be by the mode of chemical bonding, both are linked together, promote the transmission of photogenerated charge at both interfaces, be conducive to the compound reducing photo-generated carrier.
Advantage of the present invention:
One, the present invention prepares oversubscription and to fall apart α-Fe
2o
3quantum dot/nitrogen-doped graphene composite functional material, wherein α-Fe
2o
3the average grain diameter of quantum dot is only 3.2nm;
Two, the reaction condition of the inventive method is gentle, and the consersion unit adopted is simple, and required reagent is cheap, and safety non-toxic, be conducive to large-scale production;
Three, the α-Fe prepared by the present invention
2o
3the active Fe apparently higher than business of light Fenton of quantum dot/nitrogen-doped graphene composite
2o
3, to the clearance of rhodamine B up to 92%.
Accompanying drawing explanation
Fig. 1 is that α-Fe is prepared in test one
2o
3the transmission electron microscope picture of quantum dot/nitrogen-doped graphene composite;
Fig. 2 is α-Fe prepared by test one
2o
3the transmission electron microscope picture of quantum dot/nitrogen-doped graphene composite;
Fig. 3 is α-Fe prepared by test one
2o
3the x-ray photoelectron spectroscopy figure of quantum dot/nitrogen-doped graphene composite, peak 1 is the 3p track absworption peak of Fe, and peak 2 is the 1s track absworption peak of C, peak 3 is the 1s track absworption peak of N, peak 4 is the 1s track absworption peak of O, and peak 5 is the 2p track absworption peak of Fe, and peak 6 is the 2s track absworption peak of Fe;
Fig. 4 is the design sketch of rhodamine B in neutral light Fenton degradation water, and curve 1 is the effect curve of test five, and curve 2 is the effect curve of test four, and curve 3 is the effect curve of test three, and curve 4 is the effect curve of test two.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of α-Fe
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite, specifically carries out according to the following steps:
One, join in deionized water by the organic matter containing hydroxyl, mix and blend 5min ~ 10min, obtains organic solution; The aqueous solution of alkali source and inorganic iron is joined in organic solution successively, stirs 5min ~ 10min, form uniform transparent mixed liquor; Described is 1g:(0.5mL ~ 1mL containing the organic quality of hydroxyl and the volume ratio of deionized water); Described alkali source is 1:(100 ~ 200 with the organic mass ratio containing hydroxyl); The concentration of the aqueous solution of described inorganic iron is 0.05mol/L ~ 0.5mol/L; The volume of the aqueous solution of described inorganic iron is 1mL:(4.29g ~ 8.57g with the organic mass ratio containing hydroxyl);
Two, joined by graphene oxide in the uniform transparent mixed liquor that step one obtains, ultrasonic 0.3h ~ 2.0h, then stirs 2.0h ~ 4.0h, obtains stable suspension; Described graphene oxide and the organic mass ratio containing hydroxyl described in step one are 1:(750 ~ 1500);
Three, after stable suspension step 2 obtained pours hydrothermal reaction kettle into, be react 5h ~ 36h under the condition of 100 DEG C ~ 200 DEG C in temperature, naturally cool to room temperature, carry out centrifugal, then spend deionized water 3 times, 2 times are washed again with ethanol, finally dry 12h under temperature is the condition of 50 DEG C, obtains α-Fe
2o
3quantum dot/nitrogen-doped graphene composite.
The principle of present embodiment:
In present embodiment, iron ion is due to electrostatic interaction, can be adsorbed on the graphenic surface of N doping, nucleating growth; In addition, because the organic matter containing hydroxyl contains multiple hydroxyl, it can effectively be adsorbed on α-Fe
2o
3nanocrystalline surface, therefore, present embodiment adds a large amount of organic matters containing hydroxyl and makes α-Fe in preparation process
2o
3nanocrystalline surface is covered by the organic matter containing hydroxyl completely, to limit α-Fe
2o
3nanocrystalline further growth; Meanwhile, α-Fe is covered
2o
3nanocrystal surface containing the organic matter of hydroxyl can also effectively hinder nanocrystalline between reunion, and then obtain hyperfine α-Fe
2o
3quantum dot (mean size is 3.2nm), surpasses and is scattered on nitrogen-doped graphene sheet;
In composite prepared by present embodiment, α-Fe
2o
3the average grain diameter of quantum dot is 3.2nm, and within the diffusion path scope of photohole, therefore photohole can effectively arrive α-Fe
2o
3the surface of quantum dot, and then oxidative degradation rhodamine B; Due to α-Fe
2o
3quantum dot is very little, and therefore its chemism point position exposed is more, therefore can effective rhodamine B degradation; Due to α-Fe
2o
3quantum dot be growth in situ on nitrogen-doped graphene sheet, be by the mode of chemical bonding, both are linked together, promote the transmission of photogenerated charge at both interfaces, be conducive to the compound reducing photo-generated carrier.
Present embodiment advantage:
One, present embodiment is prepared oversubscription and to be fallen apart α-Fe
2o
3quantum dot/nitrogen-doped graphene composite functional material, wherein α-Fe
2o
3the average grain diameter of quantum dot is only 3.2nm;
Two, the reaction condition of present embodiment method is gentle, and the consersion unit adopted is simple, and required reagent is cheap, and safety non-toxic, be conducive to large-scale production;
Three, the α-Fe prepared by present embodiment
2o
3the active Fe apparently higher than business of light Fenton of quantum dot/nitrogen-doped graphene composite
2o
3, to the clearance of rhodamine B up to 92%.。
Detailed description of the invention two: present embodiment and detailed description of the invention one unlike: the organic matter containing hydroxyl described in step one is glycerine, sucrose, glucose or hydroxylated cellulose.Other is identical with detailed description of the invention one.
Detailed description of the invention three: one of present embodiment and detailed description of the invention one to two unlike: the alkali source described in step one is urea, ammoniacal liquor or ammonium acetate.Other is identical with one of detailed description of the invention one to two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three unlike: the inorganic iron described in step one is ferric trichloride, ferrous chloride, ferrous sulfate or ferric nitrate.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four are 1:(130 ~ 180 unlike: the described alkali source described in step one and the organic mass ratio containing hydroxyl).Other is identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five volume unlike: the aqueous solution of the described inorganic iron described in step one is 1mL:(5g ~ 7g with the organic mass ratio containing hydroxyl).Other is identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six are 1:(900 ~ 1000 unlike the organic mass ratio containing hydroxyl described in: the graphene oxide described in step 2 and step one).Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to seven unlike: after stable suspension step 2 obtained described in step 3 pours hydrothermal reaction kettle into, be react 24h under the condition of 150 DEG C in temperature, naturally cool to room temperature.Other is identical with one of detailed description of the invention one to seven.
Adopt following verification experimental verification effect of the present invention:
Test one: this test is a kind of α-Fe
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite, specifically carries out according to the following steps:
One, join in deionized water by the organic matter containing hydroxyl, mix and blend 5min, obtains organic solution; The aqueous solution of alkali source and inorganic iron is joined in organic solution successively, stirs 5min, form uniform transparent mixed liquor; Described is 1g:0.86mL containing the organic quality of hydroxyl and the volume ratio of deionized water; Described alkali source is 1:116.67 with the organic mass ratio containing hydroxyl; The concentration of the aqueous solution of described inorganic iron is 0.2mol/L; The volume of the aqueous solution of described inorganic iron is 1mL:5g with the organic mass ratio containing hydroxyl;
Two, joined by graphene oxide in the uniform transparent mixed liquor that step one obtains, ultrasonic 0.5h, then stirs 2h, obtains stable suspension; Described graphene oxide and the organic mass ratio containing hydroxyl described in step one are 1:875;
Three, after stable suspension step 2 obtained pours hydrothermal reaction kettle into, be react 24h under the condition of 150 DEG C in temperature, naturally cool to room temperature, carry out centrifugal, then spend deionized water 3 times, 2 times are washed again with ethanol, finally dry 12h under temperature is the condition of 50 DEG C, obtains α-Fe
2o
3quantum dot/nitrogen-doped graphene composite.
The organic matter containing hydroxyl described in step one is glycerine; Alkali source described in step one is urea; Inorganic iron described in step one is ferric trichloride.
Fig. 1 is α-Fe prepared by test one
2o
3the transmission electron microscope picture of quantum dot/nitrogen-doped graphene composite, Fig. 2 is α-Fe prepared by test one
2o
3the transmission electron microscope picture of quantum dot/nitrogen-doped graphene composite, as shown in Figure 1, the α-Fe of this test preparation
2o
3quantum dot/nitrogen-doped graphene composites pattern is two-dimensional sheet structure, and the outward appearance of the graphene oxide in this and step 2 is basically identical; As shown in Figure 2, the hyperfine α-Fe of this test preparation
2o
3quantum dot (mean size is 3.2nm) is dispersed on whole nitrogen-doped graphene sheet uniformly, simultaneously not obvious α-Fe that is large or that reunite on nitrogen-doped graphene sheet
2o
3quantum dot.
Fig. 3 is α-Fe prepared by test one
2o
3the x-ray photoelectron spectroscopy figure of quantum dot/nitrogen-doped graphene composite, peak 1 is the 3p track absworption peak of Fe, peak 2 is the 1s track absworption peak of C, peak 3 is the 1s track absworption peak of N, peak 4 is the 1s track absworption peak of O, and peak 5 is the 2p track absworption peak of Fe, and peak 6 is the 2s track absworption peak of Fe, this collection of illustrative plates obviously can find the absworption peak of C, O, N and Fe element, illustrate that composite prepared by test one is α-Fe
2o
3quantum dot/nitrogen-doped graphene composite.
Test two: this test is the effect test of rhodamine B in light Fenton degradation water:
The light source that this test adopts is the xenon lamp of 300W, and configures the edge filter of 400nm, and concrete steps are: by the aqueous solution of 50mL rhodamine B at (C
0=50mg/L) dark place stirs after 30min, and the pH of solution is adjusted to 7.0 by NaOH or the HCl solution then adopted, and opens xenon lamp, carries out photochemical reaction, and in test solution, the concentration of rhodamine B is along with the change in reaction time.
Test three: this test is the effect test of rhodamine B in light Fenton degradation water:
The light source that this test adopts is the xenon lamp of 300W, and configures the edge filter of 400nm, and concrete steps are: by the aqueous solution of 50mL rhodamine B at (C
0=50mg/L) dark place stirs after 30min, and the pH of solution is adjusted to 7.0 by NaOH or the HCl solution then adopted, then adds the H that 0.5mL mass concentration is 3%
2o
2the aqueous solution, opens xenon lamp, carries out photochemical reaction, and in test solution, the concentration of rhodamine B is along with the change in reaction time.
Test four: this test is the effect test of rhodamine B in light Fenton degradation water:
The light source that this test adopts is the xenon lamp of 300W, and configures the edge filter of 400nm, and concrete steps are: by 10mg business Fe
2o
3join the aqueous solution (C of 50mL rhodamine B
0=50mg/L) in, after in the dark stirring 30min, the pH of solution is adjusted to 7.0 by NaOH or the HCl solution then adopted, then adds the H that 0.5mL mass concentration is 3%
2o
2the aqueous solution, opens xenon lamp, carries out photochemical reaction, and in test solution, the concentration of rhodamine B is along with the change in reaction time.
Test five: this test is the effect test of rhodamine B in light Fenton degradation water:
The light source that this test adopts is the xenon lamp of 300W, and configures the edge filter of 400nm, and concrete steps are: by the α-Fe of 10mg test one preparation
2o
3quantum dot/nitrogen-doped graphene composite joins the aqueous solution (C of 50mL rhodamine B
0=50mg/L) in, after in the dark stirring 30min, the pH of solution is adjusted to 7.0 by NaOH or the HCl solution then adopted, then adds the H that 0.5mL mass concentration is 3%
2o
2the aqueous solution, opens xenon lamp, carries out photochemical reaction, and in test solution, the concentration of rhodamine B is along with the change in reaction time.
Fig. 4 is the design sketch of rhodamine B in neutral light Fenton degradation water, curve 1 is the effect curve of test five, and curve 2 is the effect curve of test four, and curve 3 is the effect curve of test three, curve 4 is the effect curve of test two, tests the α-Fe of a preparation as seen from Figure 4
2o
3the active Fe apparently higher than business of light Fenton of quantum dot/nitrogen-doped graphene composite
2o
3with the effect of independent hydrogen peroxide, the clearance of its rhodamine B is up to 92%.
Claims (8)
1. a α-Fe
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite, is characterized in that α-Fe
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite carries out according to the following steps:
One, join in deionized water by the organic matter containing hydroxyl, mix and blend 5min ~ 10min, obtains organic solution; The aqueous solution of alkali source and inorganic iron is joined in organic solution successively, stirs 5min ~ 10min, form uniform transparent mixed liquor; Described is 1g:(0.5mL ~ 1mL containing the organic quality of hydroxyl and the volume ratio of deionized water); Described alkali source is 1:(100 ~ 200 with the organic mass ratio containing hydroxyl); The concentration of the aqueous solution of described inorganic iron is 0.05mol/L ~ 0.5mol/L; The volume of the aqueous solution of described inorganic iron is 1mL:(4.29g ~ 8.57g with the organic mass ratio containing hydroxyl);
Two, joined by graphene oxide in the uniform transparent mixed liquor that step one obtains, ultrasonic 0.3h ~ 2.0h, then stirs 2.0h ~ 4.0h, obtains stable suspension; Described graphene oxide and the organic mass ratio containing hydroxyl described in step one are 1:(750 ~ 1500);
Three, after stable suspension step 2 obtained pours hydrothermal reaction kettle into, be react 5h ~ 36h under the condition of 100 DEG C ~ 200 DEG C in temperature, naturally cool to room temperature, carry out centrifugal, then spend deionized water 3 times, 2 times are washed again with ethanol, finally dry 12h under temperature is the condition of 50 DEG C, obtains α-Fe
2o
3quantum dot/nitrogen-doped graphene composite.
2. a kind of α-Fe according to claim 1
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite, is characterized in that the organic matter containing hydroxyl described in step one is glycerine, sucrose, glucose or hydroxylated cellulose.
3. a kind of α-Fe according to claim 1
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite, is characterized in that the alkali source described in step one is urea, ammoniacal liquor or ammonium acetate.
4. a kind of α-Fe according to claim 1
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite, is characterized in that the inorganic iron described in step one is ferric trichloride, ferrous chloride, ferrous sulfate or ferric nitrate.
5. a kind of α-Fe according to claim 1
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite, is characterized in that the alkali source described in step one is 1:(130 ~ 180 with the organic mass ratio containing hydroxyl).
6. a kind of α-Fe according to claim 1
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite, is characterized in that the volume of the aqueous solution of the inorganic iron described in step one is 1mL:(5g ~ 7g with the organic mass ratio containing hydroxyl).
7. a kind of α-Fe according to claim 1
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite, is characterized in that the organic mass ratio containing hydroxyl described in the graphene oxide described in step 2 and step one is 1:(900 ~ 1000).
8. a kind of α-Fe according to claim 1
2o
3the preparation method of quantum dot/nitrogen-doped graphene composite, after it is characterized in that stable suspension step 2 obtained described in step 3 pours hydrothermal reaction kettle into, is react 24h under the condition of 150 DEG C in temperature, naturally cools to room temperature.
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