CN102051667A - Method for studying in-situ growing process of MnMo04.H20 nanorod - Google Patents
Method for studying in-situ growing process of MnMo04.H20 nanorod Download PDFInfo
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- CN102051667A CN102051667A CN 201010602567 CN201010602567A CN102051667A CN 102051667 A CN102051667 A CN 102051667A CN 201010602567 CN201010602567 CN 201010602567 CN 201010602567 A CN201010602567 A CN 201010602567A CN 102051667 A CN102051667 A CN 102051667A
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Abstract
The invention provides a method for studying an in-situ growing process of a MnMo04.H20 nanorod. In the method, the characteristic thermography curve of the MnMo04.H20 nanorod, which is synthesized by a microemulsion method at the temperature of 298.15 K, is subjected to in-situ monitoring by a microcalorimetry at first; and the structure, topography and size of the MnMo04.H20 nanorod are represented through X-ray diffraction (XRD) and transmission electron microscope (TEM) technologies. The variation of thermopower along with time is recorded in real time through a microcalorimeter so as to acquire the thermodynamic information of the in-situ growth process of the MnMo04.H20 nanorod by combining XRD spectrums and TEM pictures, thereby studying the thermodynamic rule and growth mechanism of the growth process of the MnMo04.H20 nanorod. In the method, the high-precision high-sensitivity microcalorimeter is adopted to automatically monitor the variation process of the system in an on-line mode and simultaneously acquire the process thermodynamic information and dynamic information; and the invention provides a new method for studying on the in-situ growth process of the MnMo04.H20 nanorod, and the method can be widely applied to the study on the in-situ growth process of inorganic functional materials.
Description
Technical field
The present invention relates to a kind of inorganic functional nano material in-situ Research of growth, particularly a kind of employing high precision, highly sensitive RD496-2000 micro calorimeter research MnMoO
4H
2The method of O nanometer rod growth in situ process.
Background technology
Why nano material can grow and how to grow, how are the rule of process of growth and feature? adopt any method to obtain the information of nano material process of growth, make thermodynamics, kinetics and the growth mechanism thereof of nano material process of growth clear, sum up the feature and the rule of nano material growth, provide scientific and reasonable explanation, thereby realize the controllable growth of nano material, and then reach the regulation and control of structure and rerum natura, be the target that the nano material preparation science is pursued always.
At present, the process of growth of research nano material mainly contains following several method: (1) with classical kinetics of crystallization theory study nano material grow [Sugimoto T, Kimijima K.Journal of Physical Chemistry B.2003; 107; 10753-9], promptly institute's synthetic nano material being carried out final state (or intermediate state) under certain condition detects, characterize form, structure, composition and rerum natura, analyze by detected result, explore the growth conditions of controlledly synthesis, research growth mechanism and growth kinetics [Guo Min, Diao Peng, Wang Xindong, Cai Shengmin. the journal .2007 of University of Science ﹠ Technology, Beijing; 7; 735-8+749]; (2) with Electronic Speculum original position research nano material process of growth [a) Zhang XZ, Zhang JM, Chen L, Xu J, You LP, Yu DP.AppliedPhyscis A:Materials Science; Processing.2008; 92; 669-672.b) Stach FA, Pauzuskie PJ, Kuykendall T, Goldberger J, He RR, Yang PD.Nano Letters.2003; 3; 867-9.c) Radisic A, VereeckenPM, Hannon JB, Searson PC, Rss FM.Nano Letters.2006; 6; 238-42.d) Chou YC, Wu WW, ChengSL, Yoo B-Y, Myung N, Chen LJ, Tu KN.Nano Letters.2008; 8; 2194-9.]; (3) usefulness scanning tunnel microscope real-time monitored nano material growth [a) Skutnik PD, Sgarlata A, Nufris S, Motta N, Balzarotti A.PhysicalReview is B.2004; 69; 201309.b) Zell CA, Freyland W.Langmuir.2003; 19; 7445-50.]; (4) with the elliptical polarization diagnostic techniques growth kinetics, the character of nano material are carried out on-line monitoring [Logothetidis S, Gioti M, Patsalas P.Diamond and Related Materials.2001; 10; 117-24.]; (5) [Ryan MP.Journal of Physical Chemistry C.2008 for Lngham B, Llly BN to use coordination accelerator X ray absorption in-situ observation nanostructure nucleation and process of growth; 112; 2820-4.]; (6) with UV spectrum (UV) absorption the nano-cluster process of growth is carried out real-time online dynamics research [Mercado L, Castro W, Vicu ü a E, Briano JG, Ishikawa Y, Irizarry R, Sol á L, Castro ME.International Conference on Computational Nanoscience and Nanotechnology-ICCN.2002; 439-42.]; (7) in conjunction with original position x-ray photoelectron power spectrum the growth velocity of nanostructure is carried out on-line monitoring [Chelly R, Werckmann J, Angot T, Louis P, Bolmont D, Koulmann JJ.Thin SolidFilms.1997 with QCM (Quartz Crystal Microbalance); 294; 84-7.].
More than the problem that exists of these methods be can not be with the dynamic meticulous information of temporal variation of the non-equilibrium process of growth of common growth parameter(s) (temperature, concentration etc.) description nano material.The whole process of nano material growth promptly can't be described with certain common parameter tracking, comprise thermodynamics information, dynamic information and growth mechanism that chemical reaction, nucleating growth and pattern develop, the difference and the final different positive connection of pattern of process of growth can't be described, under many circumstances the result that the explanation of growth mechanism is just inferred.As: with the growth kinetics of XRD research nanoparticle, only spheroidal particle is suitable for and can not follows the tracks of synchronously; The growth of Electronic Speculum original position research nano material is monitored under the needed special conditions in Electronic Speculum and carried out, and is different fully with the growth actual environment of common nano material, can not be applied to general nano material process of growth research.In addition, though the original position electron microscopy can intuitively be observed the growth evolution process of nano material, but still can not obtain the thermodynamics information and the dynamic information of particle interphase interaction in the non-equilibrium process of growth of nano material; Can carry out the research of nano material growth mechanism from atom, molecular level with scanning tunnel microscope, can not obtain the thermodynamics information and the dynamic information of particle interphase interaction in the nano material process of growth, in addition, required equipment costliness, condition harshness can not be used for the nano material process of growth research under the usual conditions.
Summary of the invention
The present invention is by using the RD496-2000 micro calorimeter to MnMoO
4H
2The growth in situ process of O nanometer rod is monitored in real time, thereby obtains its growth collection of illustrative plates, in conjunction with XRD and TEM characterization technique, and research MnMoO
4H
2The thermokinetics rule and the growth mechanism of O nanometer rod growth in situ process.
Purpose of the present invention can be achieved through the following technical solutions:
Preparation microemulsion A and B get an amount of A and B and are respectively charged among large sample pond and small sample pond (Fig. 1).The small sample pond is inserted in the large sample pond, again the stainless steel reaction pond is put in the large sample pond, then the RD496-2000 micro calorimeter is put in the stainless steel reaction pond, treating after the baseline stability small sample pond broken makes microemulsion A mix with microemulsion B, by microcalorimeter record thermoelectric force over time, obtain MnMoO
4H
2The thermography curve of O nanometer rod growth in situ.With the white precipitate centrifugation that finally obtains, repeatedly wash with acetone, dehydrated alcohol and distilled water, utilize XRD and TEM technology to characterize again.With the MnMoO that obtains
4H
2The XRD figure spectrum and the TEM picture of O nanometer rod crystal combine with the thermography curve, study its growth thermokinetics rule and growth mechanism.
Compared with prior art, the present invention has following characteristics:
1, the MnMoO among the present invention
4H
2What the research of O nanometer rod growth in situ was adopted is microcalorimetry, and this method energy automatization ground on-line monitoring system change procedure can provide process thermodynamics information and dynamic information simultaneously.
2, the present invention carries out in the RD496-2000 micro calorimeter, this instrument to solvent property, spectral quality and the electrical properties etc. of system without any condition restriction.
3, the present invention can be widely used in the research of other inorganic functional material growth in situ processes.
Description of drawings
The photo in stainless steel reaction pond, large sample pond and the small sample pond of development voluntarily that Fig. 1 uses for the research of the invention process growth in situ;
The thermography graphic representation that Fig. 2 obtains for the embodiment of the invention 1;
Fig. 3 is the MnMoO of preparation
4H
2The TEM figure of O nanometer rod crystal;
The MnMoO that Fig. 4 makes for the inventive method
4H
2The XRD figure spectrum of O nanometer rod.
Embodiment
The invention will be further described below in conjunction with specific embodiment, and the description of embodiment is only for ease of understanding the present invention, but not to the restriction of the present invention's protection.
Embodiment 1
Preparation comprises 0.1mol/L MoO
4 2-Microemulsion A, wherein the ratio P of the amount of substance of n-Octanol and alkyl polyoxyethylene (10) ether is 2.57, the amount of substance of water and alkyl polyoxyethylene (10) ether is 10 than ω, all the other are oil phase content; Make corresponding each component concentration Mn consistent with microemulsion A
2+Microemulsion B.Get pack into the big glass sample pond of diameter 1.2cm, high 6.5cm of 1mL microemulsion A, pack into the little glass sample pond of diameter 1.0cm, high 4.5cm of 1mL microemulsion B, the small sample pond is inserted in the large sample pond, again the stainless steel reaction pond is put in the large sample pond, then the RD496-2000 micro calorimeter is put in the stainless steel reaction pond, treat after the baseline stability small sample pond broken that microemulsion A is mixed with microemulsion B, by microcalorimeter record thermoelectric force over time, MnMoO when obtaining t=24h
4H
2The thermography curve (Fig. 2) of O nanometer rod crystal growth in situ process.Whole process is carried out under 298.15K in the calorimeter, and the reaction times is 24 hours.With the white precipitate centrifugation that obtains, repeatedly wash removing unnecessary tensio-active agent and mineral ion with acetone, dehydrated alcohol and distilled water again, thereby obtain wide about 70nm, grow to the MnMoO of 4 μ m
4H
2O nanometer rod (Fig. 3).
Claims (4)
1. study MnMoO for one kind
4H
2The novel method of O nanometer rod growth in situ process is characterized in that this method is to adopt high precision, highly sensitive RD496-2000 micro calorimeter to MnMoO
4H
2The growth in situ of O nanometer rod dynamically carries out real time on-line monitoring, obtains MnMoO simultaneously
4H
2The thermokinetics information of O nanorod growth process in conjunction with XRD and TEM characterization technique, is studied the thermokinetics rule and the growth mechanism of its process of growth;
2. whole process is carried out under 298.15K in the calorimeter, and the reaction times is 24 hours;
3. with the white precipitate centrifugation that obtains in the claim 2, repeatedly wash, utilize XRD and TEM technology to characterize again with acetone, dehydrated alcohol and distilled water;
4. with the MnMoO that obtains in the claim 3
4H
2O crystalline XRD figure spectrum and TEM picture combine with the thermography curve, study the thermokinetics rule and the growth mechanism of its process of growth.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445274A (en) * | 2008-12-25 | 2009-06-03 | 广西民族大学 | Method for preparing octahedral barium molybdate |
| CN101445273A (en) * | 2008-12-25 | 2009-06-03 | 广西民族大学 | Method for preparing MnMoO4.H2O nano-rod |
| CN101650324A (en) * | 2009-08-21 | 2010-02-17 | 重庆大学 | Device for testing heat map spectra of microbial biochemical reaction |
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- 2010-12-23 CN CN 201010602567 patent/CN102051667A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445274A (en) * | 2008-12-25 | 2009-06-03 | 广西民族大学 | Method for preparing octahedral barium molybdate |
| CN101445273A (en) * | 2008-12-25 | 2009-06-03 | 广西民族大学 | Method for preparing MnMoO4.H2O nano-rod |
| CN101650324A (en) * | 2009-08-21 | 2010-02-17 | 重庆大学 | Device for testing heat map spectra of microbial biochemical reaction |
Non-Patent Citations (1)
| Title |
|---|
| 《物理化学学报》 20091231 米艳等 CaMoO4微晶生长过程的原位微量热法研究 2422-2426 1-4 第25卷, 第12期 * |
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Application publication date: 20110511 |