CN102674474A - Method for preparing two-dimensional Fe3O4 nano material - Google Patents
Method for preparing two-dimensional Fe3O4 nano material Download PDFInfo
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- CN102674474A CN102674474A CN2011103890694A CN201110389069A CN102674474A CN 102674474 A CN102674474 A CN 102674474A CN 2011103890694 A CN2011103890694 A CN 2011103890694A CN 201110389069 A CN201110389069 A CN 201110389069A CN 102674474 A CN102674474 A CN 102674474A
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Abstract
The invention discloses a method for preparing a two-dimensional Fe3O4 nano material. The method comprises the following steps of A, preparing an egg white solvent; B, preparing the two-dimensional Fe3O4 nano material; and C, washing. Compared with the prior art, the method has the advantages that the synthetic method of the Fe3O4 nano material is simple and novel, can be accomplished by one step, is easily operated and high in repeatability; the two-dimensional profile of the material can be controlled under the condition that egg white is used; the size in the same dimension can be controlled; and the method can be widely used for preparing other two-dimensional metallic oxides. Besides, products prepared by the method have the characteristics of high purity, uniform size distribution and the like.
Description
Technical field:
The invention belongs to this technical field of magnetic metal oxide preparation of nanomaterials, a kind of preparation two dimension Fe of simple novelty is provided
3O
4The method of nano material.
Technical background:
From the development of modern biotechnology, be not difficult to find that a lot of biosystems itself is exactly some perfect nano-machines.And in fact, biotechnological means has become one of method of leading to nanotechnology.It can combine with diverse discipline, promotes each subject development, also can in other subject development progress, reach the perfect of self.At occurring in nature, many biologies special inorganic materials of complex functionality is voluntarily arranged, such as Magnetictaxis bacteria, fish; Mollusk, sea urchin, sponge; Diatom etc., and the pair cell behavior that deeply helps of the fine structure understanding of life own is better regulated and control, the development of emerging research field promoted.More because countless specific like this existence in the Nature, increasing specific biological molecule come to light and be applied to inorganic materials preparation and synthetic in, commonly used just have protein, peptide, a DNA etc.Select suitable protein; Peptide, DNA wait when preparing inorganic materials, the reaction conditions milder (compared to the compound method of routine) that becomes; Such as neutral or approach in the neutral aqueous solution, and the perfection structure that just can reach material at ambient temperature.Their existence makes the energy of reaction needed input reduce, and does not need non-natural reaction solvent (such as organic solvent) simultaneously, though also be reflected at get final product under the condition of more " green " so that reaction carry out and accomplish.Simultaneously through to protein, peptide, the size of DNA etc., the structure of pattern can be realized the structure of the corresponding aspect of material, thereby another available approach efficiently is provided for the exquisite design and the structure of material.The more noticeable protein that is to use, peptide, DNA etc. also possibly generate the material of high-efficiency multi-function, have the material of biological property (being similar to organized enzyme etc.) such as some, and realize self-assembly of material or the like.Kinds of protein is various, very strange in the Nature simultaneously, has more more superior character waiting for coming to light and is developed.The functional group that exists a lot of being easy to combine in these biomolecules with mineral ion.Such as bovine serum albumin with-OH ,-NH group, collagen fibers with-OH ,-COOH and-NH
2Or the like, these groups are easy to and Cr
3+, Al
3+, Zr
4+, Ti
4+, Ag
+Combine Deng mineral ion.When giving some reductive agents, just can obtain the inorganic metal material of corresponding biomolecular structure or the material that inorganic metal combines with biomolecules.Then discover,, change change pH values or ionic strength etc. and can realize the biomolecules self-assembly through Intermolecular Forces.
Effort has in this respect been made a lot, and is single with regard to biomolecules self-assembly synthetic nano material, and certain achievement has been arranged, and what obtain usually is 0 dimension material, but 1 dimension, 2 dimensions, the material of 3 dimensions still seldom, defective is:
Though 1 has realized the self-assembly of some biomolecules, also well do not combine with the synthetic of inorganic materials.Even the nano material of some specific appearance structure is achieved through the use of biomolecules.
2, mostly synthetic is the corresponding material that obtains after the biomineralization, like silicon.Though some precious metals and some MOXs also are synthesized, be not very general, and the synthetic nanoparticle account for sizable ratio.The ubiquity of the application of experimental technique awaits to explore and find.
Summary of the invention:
A kind of technical problem to be solved by this invention provides the two-dimentional Fe of a kind of simple preparation
3O
4The method of nano material.
The technical scheme of technical solution problem of the present invention is: a kind of preparation Fe
3O
4The method of two-dimensional nano material,
A, preparation egg white solvent:
Room temperature descend with in advance from egg the egg white of separator well under the condition of stirring of limit, add entry, let egg white in water, dissolve 1-12h, isolate undissolved white mass with whizzer then, get supernatant as the egg white solvent; The volume ratio of water and egg white is 1: 0.05-0.7;
B, prepare two-dimentional Fe
3O
4Nano material:
Ferric sulfate is joined in the above-mentioned egg white solvent, stir, obtain orange-yellow solution, the mass/volume of ferric sulfate and egg white solvent is than (g/ml)=0.013-0.5/10
Orange-yellow solution is poured in the ethanolic soln that mass concentration is 0.01-0.04g/ml cetyl trimethylammonium bromide CTAB, stirred after 10-20 minute, obtain the sedimentary solution of yellow-white; Adding mass concentration again is the 50-80% Hydrazine Hydrate 80; Or mass concentration is the 0.008-0.02g/ml urea soln, stirs after 10-20 minute, and the above-mentioned reaction soln for preparing is transferred in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate; Sealing, reaction is 12-24 hour in 120-200 ℃ baking oven;
The mass ratio of ferric sulfate, cetyl trimethylammonium bromide, urea=1: 3.2-10.2: 2.5-5.6
Ferric sulfate and mass concentration are that the mass/volume of 50-80% Hydrazine Hydrate 80 is than (g/ml)=0.013/5-0.5/5
C, washing: after the cooling that product is centrifugal, collecting precipitation with absolute ethanol washing 2-3 time, promptly obtains 2 dimension Fe
3O
4Nano material.
In described operation steps, use CTAB as the morphology control agent, not growing of other directions protected in its existence, makes material only extend to two-dimensional directional.
Because of protein has complicated quaternary structure, when using the egg white solvent, need to use urea as reactor drum, 50% and 80% Hydrazine Hydrate 80 breaks hydrogen bond etc., thus the size of control material and thickness.
Present method prepares two-dimentional Fe
3O
4Nano material uses egg white as reaction medium, and is cheap and easy to get, and environmental protection.Present method prepares uses CTAB as tensio-active agent and morphology control agent in the process, the Hydrazine Hydrate 80 of use different concns and urea are as the key point agent and the Fe of egg white
3+Reductive agent.
While two-dimentional Fe of the present invention
3O
4But the nano material effective application is in fuel cell, the comparable Precious Metals-Gold of its half-wave potential, and its preparation method is simple more than gold, cost is lower than gold, and productive rate is big more than gold.
The present invention compared with prior art, Fe
3O
4The compound method of nano material is simply novel, and a step accomplishes, and is easy to operate; Circulation ratio is strong, under the situation of using egg white, has realized that the pattern of material two dimension is controlled; Also realize the controllable size in tieing up together, and possibly generally be applicable to the preparation of other two-dimensional metallic oxide compounds.The product that makes through present method has characteristics such as purity height and even size distribution.
Description of drawings:
Figure one is the two-dimentional Fe that embodiment 3 makes
3O
4Nano material sem (SEM) photo, figure a, figure b are different multiplying.
Figure two is two-dimentional Fe that embodiment 3 makes
3O
4Nano material transmission electron microscope (TEM) photo, figure a, figure b are different multiplying.
Figure three is two-dimentional Fe that embodiment 3 makes
3O
4The photo of the linear time base sweep volt-ampere curve of nano material.
Embodiment:
Be the non-limiting preparation embodiment of the present invention below, the present invention further described through these embodiment.
Embodiment 1:
A, prepare the egg white solvent: room temperature descend with in advance from egg the egg white of separator well get 2.5mL in beaker, under the condition of stirring of limit, add 10mL water.Let egg white in water, dissolve 1h, isolate undissolved white mass with whizzer then.Getting rest solution is the egg white solvent.
B, prepare two-dimentional Fe
3O
4Nano material: the ferric sulfate that takes by weighing 0.025g joins in the egg white solvent of 12.5mL, stirs, and obtains orange-yellow solution.
Get in the absolute ethyl alcohol that 0.1g CTAB is dissolved in 5mL.
Orange-yellow solution is slowly poured in the ethanol that is dissolved with CTAB, stirred after 15 minutes, obtain the sedimentary solution of yellow-white, slowly add the 5mL50% Hydrazine Hydrate 80 again.Stir after 15 minutes being transferred in the stainless steel cauldron of 30mL polytetrafluoroethylsubstrate substrate sealing in the above-mentioned reaction soln for preparing.Reaction is 12 hours in 120 ℃ baking oven.
C, washing: after the cooling that product is centrifugal, collecting precipitation with absolute ethanol washing 2-3 time, promptly obtains two-dimentional Fe
3O
4Nano material.Sheet is little and thick.
Embodiment 2:
A, preparation egg white solvent:
Room temperature descend with in advance from egg the egg white of separator well get 3mL in beaker, under the condition of stirring of limit, add 10mL water.Let egg white in water, dissolve 12h, isolate undissolved white mass with whizzer then.Getting rest solution is reaction solvent.
B, prepare two-dimentional Fe
3O
4Nano material:
The ferric sulfate that takes by weighing 0.015g joins in the above-mentioned egg white solution, stirs, and obtains orange-yellow solution.
Get in the absolute ethyl alcohol that 0.08g CTAB is dissolved in 5mL.
Orange-yellow solution is slowly poured in the ethanol that is dissolved with CTAB, stirred after 15 minutes, obtain the sedimentary solution of yellow-white, slowly add 5mL 80% Hydrazine Hydrate 80 again.Stir after 15 minutes being transferred in the stainless steel cauldron of 30mL polytetrafluoroethylsubstrate substrate sealing in the above-mentioned reaction soln for preparing.Reaction is 24 hours in 180 ℃ baking oven.
C, washing: after the cooling that product is centrifugal, collecting precipitation with absolute ethanol washing 2-3 time, promptly obtains two-dimentional Fe
3O
4Nano material, sheet is little evenly, about thick 10nm.
Embodiment 3:
A, preparation egg white solvent:
Room temperature descend with in advance from egg the egg white of separator well get 3mL in beaker, under the condition of stirring of limit, add 10mL water.Let egg white in water, dissolve 1h, isolate undissolved white mass with whizzer then.Getting rest solution is reaction solvent.
B, prepare two-dimentional Fe
3O
4Nano material:
The ferric sulfate that takes by weighing 0.015g joins in the above-mentioned egg white solution, stirs, and obtains orange-yellow solution.
Get in the absolute ethyl alcohol that 0.16g CTAB is dissolved in 5mL.
Orange-yellow solution is slowly poured in the ethanol that is dissolved with CTAB, stirred after 15 minutes, obtain the sedimentary solution of yellow-white, slowly add 5mL urea soln (urea of 0.04g is dissolved in the water of 5mL) again.Stir after 15 minutes being transferred in the stainless steel cauldron of 30mL polytetrafluoroethylsubstrate substrate sealing in the above-mentioned reaction soln for preparing.Reaction is 24 hours in 180 ℃ baking oven.
C, washing: after the cooling that product is centrifugal, collecting precipitation with absolute ethanol washing 2-3 time, promptly obtains two-dimentional Fe
3O
4Nano material, sheet reach micron order and very thin and curling greatly.
2, electrochemical property test:
Get the two-dimentional Fe of preparation
3O
4Nano material 4mg is scattered in the ethanolic soln of 1mL; Get 20 μ L and drip on the SCE that cleans up, dripping the naphthols of 10 μ L behind the certain hour, treat that electrode is done after; In the KOH of 1M solution, detect with linear time base sweep volt-ampere curve method, the rotating speed of disk electrode is 1000 commentaries on classics.The evaluation method of performance is half-wave potential and current corresponding density thereof.
Shown in figure three: the half-wave potential of this material is at-0.40V, with the half-wave potential-0.43V of gold near and calibration.It is the pretty good non-noble metal fuel cell material of performance.
Embodiment 4:
A, preparation egg white solvent:
Room temperature descend with in advance from egg the egg white of separator well get 4mL in beaker, under the condition of stirring of limit, add 10mL water.Let egg white in water, dissolve 12h, isolate undissolved white mass with whizzer then.Getting rest solution is reaction solvent.
B, prepare two-dimentional Fe
3O
4Nano material:
The ferric sulfate that takes by weighing 0.5000g joins in the above-mentioned egg white solution, stirs, and obtains orange-yellow solution.
Get in the absolute ethyl alcohol that 0.2g CTAB is dissolved in 5mL.
Orange-yellow solution is slowly poured in the ethanol that is dissolved with CTAB, stirred after 15 minutes, obtain the sedimentary solution of yellow-white, slowly add the 7mL50% Hydrazine Hydrate 80 again, or 80% Hydrazine Hydrate 80, or urea soln (urea of 0.1g is dissolved in the water of 7mL).Stir after 15 minutes being transferred in the stainless steel cauldron of 30mL polytetrafluoroethylsubstrate substrate sealing in the above-mentioned reaction soln for preparing.Reaction is 12 hours in 180 ℃ baking oven.
C, washing: after the cooling that product is centrifugal, collecting precipitation with absolute ethanol washing 2-3 time, promptly obtains two-dimentional Fe
3O
4Nano material, sheet medium (Hydrazine Hydrate 80) or big (urea) and thick.
Embodiment 5: Comparative Examples 1
A, preparation egg white solvent:
Room temperature descend with in advance from egg the egg white of separator well get 3mL in beaker, under the condition of stirring of limit, add 10mL water.Let egg white in water, dissolve 1h, isolate undissolved white mass with whizzer then.Getting rest solution is reaction solvent.
B, preparation Fe
3O
4Nano material:
The ferric sulfate that takes by weighing 0.015g joins in the above-mentioned egg white solution, stirs, and obtains orange-yellow solution.
Get the absolute ethyl alcohol of 5mL.
Orange-yellow solution is slowly poured in the ethanol that does not add CTAB, stirred after 15 minutes, obtain the sedimentary solution of yellow-white, slowly add 5mL urea soln (urea of 0.04g is dissolved in the water of 5mL) again.Stir after 15 minutes being transferred in the stainless steel cauldron of 30mL polytetrafluoroethylsubstrate substrate sealing in the above-mentioned reaction soln for preparing.Reaction is 24 hours in 180 ℃ baking oven.
C, washing: after the cooling that product is centrifugal, collecting precipitation with absolute ethanol washing 2-3 time, promptly obtains particulate state Fe
3O
4Nano material, no sheet.
Embodiment 6: Comparative Examples 2
A, ready reaction solvent:
Get 10mL water as reaction solvent;
B, preparation Fe
3O
4Nano material:
The ferric sulfate that takes by weighing 0.015g joins in the above-mentioned reaction solvent water, stirs, and obtains xanchromatic solution.
Get in the absolute ethyl alcohol that 0.16g CTAB is dissolved in 5mL.
Yellow solution is slowly poured in the ethanol that is dissolved with CTAB, stirred after 15 minutes, obtain the sedimentary solution of yellow-white, slowly add 5mL urea soln (urea of 0.04g is dissolved in the water of 5mL) again.Stir after tens minutes being transferred in the stainless steel cauldron of 30mL polytetrafluoroethylsubstrate substrate sealing in the above-mentioned reaction soln for preparing.Reaction is 24 hours in 180 ℃ baking oven.
C, washing: after the cooling that product is centrifugal, collecting precipitation with absolute ethanol washing 2-3 time, promptly obtains particulate state Fe
3O
4Nano material, and big and inhomogeneous.
Claims (3)
1. one kind prepares Fe
3O
4The method of two-dimensional nano material is characterized in that: comprise following operation:
A, preparation egg white solvent:
Room temperature descend with in advance from egg the egg white of separator well under the condition of stirring of limit, add entry, let egg white in water, dissolve 1-12h, isolate undissolved white mass with whizzer then, get supernatant as the egg white solvent; The volume ratio of water and egg white is 1: 0.05-0.7;
B, prepare two-dimentional Fe
3O
4Nano material:
Ferric sulfate is joined in the above-mentioned egg white solvent, stir, obtain orange-yellow solution, the mass/volume of ferric sulfate and egg white solvent is than (g/ml)=0.013-0.5/10;
Orange-yellow solution is poured in the ethanolic soln that mass concentration is 0.01-0.04g/ml cetyl trimethylammonium bromide CTAB, stirred after 10-20 minute, obtain the sedimentary solution of yellow-white; Adding mass concentration again is the 50-80% Hydrazine Hydrate 80; Or mass concentration is the 0.008-0.02g/ml urea soln, stirs after 10-20 minute, and the above-mentioned reaction soln for preparing is transferred in the stainless steel cauldron of polytetrafluoroethylsubstrate substrate; Sealing, reaction is 12-24 hour in 120-200 ℃ baking oven;
C, washing: after the cooling that product is centrifugal, collecting precipitation with absolute ethanol washing 2-3 time, promptly obtains 2 dimension Fe
3O
4Nano material.
2. a kind of preparation Fe according to claim 1
3O
4The method of two-dimensional nano material,, it is characterized in that: the mass ratio of described ferric sulfate, cetyl trimethylammonium bromide, urea=1: 3.2-10.2: 2.5-5.6.
3. a kind of preparation Fe according to claim 1
3O
4The method of two-dimensional nano material,, it is characterized in that: described ferric sulfate and mass concentration are that the mass/volume of 50-80% Hydrazine Hydrate 80 is than (g/ml)=0.013/5-0.5/5.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103771536A (en) * | 2014-02-11 | 2014-05-07 | 济南大学 | Ferroferric oxide rhombic dodecahedron particles and preparation method thereof |
CN114751484A (en) * | 2022-05-12 | 2022-07-15 | 东北电力大学 | Alga removing method of ferroferric oxide photo-thermal nano material |
Citations (1)
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CN101026030A (en) * | 2006-12-26 | 2007-08-29 | 安徽师范大学 | Magnetic nano chain preparation and use method |
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Patent Citations (1)
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CN101026030A (en) * | 2006-12-26 | 2007-08-29 | 安徽师范大学 | Magnetic nano chain preparation and use method |
Non-Patent Citations (2)
Title |
---|
BAOYOU GENG ET AL.: "Egg albumin as a nanoreactor for growing single-crystalline Fe3O4 nanotubes with high yields", 《CHEM. COMMUN.》, 1 October 2008 (2008-10-01), pages 5773 - 5775 * |
李小东等: "高分散度Fe3O4 纳米球的粒径控制合成及磁性能", 《功能材料》, vol. 40, no. 7, 31 December 2009 (2009-12-31), pages 1233 - 1236 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103771536A (en) * | 2014-02-11 | 2014-05-07 | 济南大学 | Ferroferric oxide rhombic dodecahedron particles and preparation method thereof |
CN114751484A (en) * | 2022-05-12 | 2022-07-15 | 东北电力大学 | Alga removing method of ferroferric oxide photo-thermal nano material |
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Application publication date: 20120919 |