CN102502837B - Method for preparing ultrathin lanthanum molybdate nano sheet material - Google Patents
Method for preparing ultrathin lanthanum molybdate nano sheet material Download PDFInfo
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- CN102502837B CN102502837B CN 201110347394 CN201110347394A CN102502837B CN 102502837 B CN102502837 B CN 102502837B CN 201110347394 CN201110347394 CN 201110347394 CN 201110347394 A CN201110347394 A CN 201110347394A CN 102502837 B CN102502837 B CN 102502837B
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Abstract
The invention provides a method for preparing an ultrathin lanthanum molybdate nano sheet material. The micro structure of the nano structure is controlled by adopting a cetyl trimethyl ammonium bromide aided microwave radiation technology, ammonium molybdate and lanthanum nitrate are used as initial reaction raw materials, distilled water is used as a solvent, and cetyl trimethyl ammonium bromide is used as a structure directing agent. The synthesized ultrathin lanthanum molybdate nano sheet material has smooth surface and high crystallization degree, the thickness of the material is only 5 to 15 nanometers, the obtained product has large specific surface area, and the product is gathered together to form a three-dimensional network structure. According to the synthesis system, the microwave radiation energy is favorable for exerting the effect of the structure directing agent, so that the inner part of the reaction system is heated quickly and uniformly, the reaction time is remarkably shortened, the yield of unit time is improved, the preparation cost is reduced, and the composition and the structure of the product can be effectively and conveniently regulated and controlled. Due to the characteristics of large specific surface area, regular structure and the like, the ultrathin lanthanum molybdate nano sheet material obtained by adopting the technology has potential application value in the fields of electrochemistry, optics, catalysis, energy environment protection and the like.
Description
[technical field]: the preparation method who the invention belongs to synthetic field, particularly a kind of ultrathin lanthanum molybdate nano sheet material of inorganic nano material.
[background technology]: at present, develop the technology of various informative nano materials both at home and abroad, require particularly to adopt the auxiliary traditional preparation method of soft template to come the material of regulate shape novelty with the harshness that satisfies in applied research.Especially, cetyl trimethylammonium bromide (CTAB) is introduced in the nanostructure hierarchy of control because having good absorption and complex ability.This soft template the nano material nucleus form and developmental process in, can preferentially be adsorbed in particular crystal plane and produce strong sterically hindered and electrostatic adhesion effect, implementation rule self-assembly effect and reach the purpose of dominant growth and adjusting size.
The lanthanum molybdate nano material has unique physics, chemical property, therefore in fields such as electrochemistry, optics, catalysis, the energy, environment protection, important using value is arranged all as the important component part in the molybdenum based nano-material.As everyone knows, the macro property of material and its microscopic appearance are closely related.With regard to the lanthanum molybdate material, existing its microscopic appearance of bibliographical information is mainly (as: N.Zhang, W.B.Bu, the Y.P.Xu such as bulk, particulate state, flower-shaped, tubulose or taper, D.Y.Jiang, J.L.Shi, J.Phys.Chem.C, 2007,111 (13), 5014; W.B.Bu, Y.P.Xu, N.Zhang, H.R.Chen, Z.L.Hua, J.L.Shi, Langmuir, 2007,23 (17), 9002; CN 101358130A; CN 101376527B).But also having a lot of work to carry out in a deep going way aspect rapidly and efficiently synthesizing, and less about the document of two-dimentional pure phase lanthanum molybdate material preparation, particularly adopt the report of the synthetic super-thin sheet-shaped lanthanum molybdate nano material of soft template auxiliary law still less.Therefore, it is very necessary providing a kind of high, the easy and simple to handle and practical method of reaction efficiency to prepare ultrathin lanthanum molybdate nano sheet material.For the problems referred to above, patent of the present invention provides a kind of preparation method of ultrathin lanthanum molybdate nano sheet material, and it is take cetyl trimethylammonium bromide as soft template, and the type of heating of applied microwave radiation has prepared lanthanum molybdate ultrathin nanometer chip architecture.This synthetic method is effectively to control the microtexture of material, and the internal relation of analysing in depth between two-dimensional nano material small-size effect and over-all properties has been established necessary working foundation.
[summary of the invention]: the summary of the invention of this patent is to provide a kind of preparation method of ultrathin lanthanum molybdate nano sheet material, it is take cetyl trimethylammonium bromide as soft template, utilize the carry out microwave radiation heating system and pass through to optimize reaction conditions, even thickness, ganoid super-thin sheet-shaped lanthanum molybdate nano material have successfully been synthesized, realize the effective control to product composition and structure, provide condition for promoting material property.
[technical scheme of the present invention]: the invention provides a kind of preparation method of ultrathin lanthanum molybdate nano sheet material, it adopts cetyl trimethylammonium bromide assisted microwave synthesis radiotechnology, controls the microtexture of nano material, and technical scheme is as follows:
The first, with La (NO
3)
36H
2O lanthanum nitrate and cetyl trimethylammonium bromide are to join in distilled water at 10: 1 according to mol ratio, and stir, and are mixed with homogeneous mixed solution;
The second, separately prepare 0.0014mol/L ammonium molybdate (NH
4)
6Mo
7O
24Solution also joins in the mixing solutions that the first step configures, and then fully stirs 10 minutes, and reaction raw materials is fully mixed, and forms precursor solution;
Three, the precursor solution that step 2 is obtained slowly is transferred in the normal pressure microwave radiation reactor and acts on 30 minutes;
Four, with the cotton-shaped product of gained through centrifugation, with distilled water wash 3～5 times to neutral to remove unnecessary by product, then under 60 ℃ of isoperibol conditions dry 24 hours, and obtain ultrathin lanthanum molybdate nano sheet material, sample was accredited as La through phase
2MoO
6And La
2Mo
4O
15Mixed phase.
In described lanthanum nitrate and cetyl trimethylammonium bromide mixing solutions, the volumetric molar concentration of lanthanum nitrate is 0.0100mol/L, and the volumetric molar concentration of cetyl trimethylammonium bromide is 0.0010 mol/L.
Smooth surface, the degree of crystallinity of described ultrathin lanthanum molybdate nano sheet material are high, and thickness is only 5～15 nanometers, and the products therefrom specific surface area is large, form the 3 D stereo network structure and flock together each other.
[advantage of the present invention and effect]: patent of the present invention provides a kind of preparation method of ultrathin lanthanum molybdate nano sheet material, have remarkable advantage and beneficial effect: at first, the employing cetyl trimethylammonium bromide is structure directing agent, it is in lanthanum molybdate material nucleation and process of growth, can effectively lead and nanocrystallinely assemble according to two-dimentional orientation, thereby reach dominant growth and regulate the purpose of product size; Secondly, microwave radiation energy makes the inner heating of reaction system rapidly and evenly, significantly Reaction time shorten, improve the unit time productive rate, reduce preparation cost, thereby can efficiently regulate and control easily product composition and structure; At last, ultrathin lanthanum molybdate nano sheet material all has huge potential using value because of characteristics such as specific surface area is large, compound with regular structure in fields such as electrochemistry, optics, catalysis, energy environment protections.
[description of drawings]:
Fig. 1 is low power scanning electronic microscope (SEM) figure of lanthanum molybdate ultrathin nanometer sheet
Fig. 2 is the high power SEM figure of lanthanum molybdate ultrathin nanometer sheet
[embodiment]:
Embodiment: preparation method and the structural characterization of lanthanum molybdate ultrathin nanometer sheet
Under room temperature, with La (NO
3)
36H
2The mixing solutions of O lanthanum nitrate and cetyl trimethylammonium bromide, and stir, wherein the volumetric molar concentration of lanthanum nitrate is that the volumetric molar concentration of 0.0100mol/L solution, cetyl trimethylammonium bromide is 0.0010mol/L; Ammonium molybdate (the NH of another preparation 0.0014mol/L
4)
6Mo
7O
24Solution also joins in above-mentioned mixing solutions, continues fully to stir 10 minutes, and reaction raw materials is mixed, and forms the homogeneous phase precursor; The precursor that obtains is transferred in the normal pressure microwave radiation reactor acts on 30 minutes; At last with the cotton-shaped product centrifugation of gained, with distilled water wash 5 times to neutral to remove unnecessary by product, then under 60 ℃ of isoperibol conditions dry 24 hours, obtain ultrathin lanthanum molybdate nano sheet material, sample is accredited as La through phase
2MoO
6And La
2Mo
4O
15Mixed phase.Product low power SEM test (Fig. 1) result shows: product is the sheet structure of even thickness, and these nanometer sheet are cross-linked to each other together and form dimensional network structure; The nanometer sheet smooth surface, the degree of crystallinity that form as can be known these three-dimensional structures by the further observation analysis of high power SEM (Fig. 2) are high, and thickness is only 5～15 nanometers.
Claims (1)
1. the preparation method of a ultrathin lanthanum molybdate nano sheet material, it adopts cetyl trimethylammonium bromide assisted microwave synthesis radiotechnology, controls the microtexture of nano material, and technical scheme is as follows:
The first, with La (NO
3)
36H
2O lanthanum nitrate and cetyl trimethylammonium bromide are to join in distilled water at 10: 1 according to mol ratio, and stir, and are mixed with homogeneous mixed solution; In lanthanum nitrate and cetyl trimethylammonium bromide mixing solutions, the volumetric molar concentration of lanthanum nitrate is 0.0100mol/L, and the volumetric molar concentration of cetyl trimethylammonium bromide is 0.0010 mol/L;
The second, separately prepare 0.0014mol/L ammonium molybdate (NH
4)
6Mo
7O
24Solution also joins in the mixing solutions that the first step configures, and then fully stirs 10 minutes, and reaction raw materials is fully mixed, and forms precursor solution;
Three, the precursor solution that step 2 is obtained slowly is transferred in the normal pressure microwave radiation reactor and acts on 30 minutes;
Four, with the cotton-shaped product of gained through centrifugation, with distilled water wash 3～5 times to neutral to remove unnecessary by product, then under 60 ℃ of isoperibol conditions dry 24 hours, and obtain ultrathin lanthanum molybdate nano sheet material, sample was accredited as La through phase
2MoO
6And La
2Mo
4O
15Mixed phase; Smooth surface, the degree of crystallinity of ultrathin lanthanum molybdate nano sheet material are high, and thickness is only 5～15 nanometers, and the products therefrom specific surface area is large, form the 3 D stereo network structure and flock together each other.
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| CN102502837B true CN102502837B (en) | 2013-11-06 |
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| CN107093758A (en) * | 2017-04-18 | 2017-08-25 | 合肥学院 | A kind of lanthanum molybdate-based intermediate temperature solid oxide fuel cell electrolyte and preparation method thereof |
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| CN104384527B (en) * | 2014-12-10 | 2016-06-01 | 黑龙江大学 | The preparation method of the two-dimentional transition metal/metal oxides mixed phase nanometer sheet of a kind of self-supporting |
| CN106115782B (en) * | 2016-06-17 | 2017-07-18 | 天津大学 | A kind of ultra-thin sheet material of the rare earth molybdate of morphology controllable and preparation method thereof |
| CN106328916B (en) * | 2016-09-27 | 2019-05-31 | 伍伦贡大学 | A kind of lithium vanadate Li3VO4The microwave radiation preparation of nano-hollow ball |
| CN106356522B (en) * | 2016-09-27 | 2019-07-02 | 苏州科技大学 | A kind of electrochemically stable efficient storage lithium Li3VO4The low-temperature microwave synthetic method of hollow Nano cube |
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| CN102161509B (en) * | 2011-02-12 | 2013-04-03 | 河北联合大学 | Method for synthesizing metal molybdate micron/nano materials by adopting microwave radiation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107093758A (en) * | 2017-04-18 | 2017-08-25 | 合肥学院 | A kind of lanthanum molybdate-based intermediate temperature solid oxide fuel cell electrolyte and preparation method thereof |
| CN107093758B (en) * | 2017-04-18 | 2020-02-11 | 合肥学院 | Lanthanum molybdate based medium-temperature solid oxide fuel cell electrolyte material and preparation method thereof |
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