CN102417206B - Preparation method of NaV2O5 crystal material with right angle morphology - Google Patents
Preparation method of NaV2O5 crystal material with right angle morphology Download PDFInfo
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- CN102417206B CN102417206B CN 201110252199 CN201110252199A CN102417206B CN 102417206 B CN102417206 B CN 102417206B CN 201110252199 CN201110252199 CN 201110252199 CN 201110252199 A CN201110252199 A CN 201110252199A CN 102417206 B CN102417206 B CN 102417206B
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Abstract
The invention relates to a preparation method of a NaV2O5 crystal material with right angle morphology. The method comprises the following steps: a), dissolving an aromatic acid organic matter in water, adding a sodium hydroxide solution under the condition of stirring at room temperature, adding a solvent, and stirring for 40-60 minutes at room temperature so as to obtain an evenly mixed solution; b), adding ammonium metavanadate in the mixture so as to obtain a yellow and transparent mixed liquid, transferring the mixture into a stainless steel reaction kettle with a polytetrafluoroethylene lining after stirring for 3 hours, and then placing the reaction kettle in a constant-temperature drying oven of 150-200 DEG C to age for 2-60 days; and c), taking out and filtering the mixture finally obtained in the step b), drying the mixture in the constant-temperature drying oven of 40-60 DEG C so as to finally obtain the NaV2O5 crystal material with a right angle L shape. In the preparation method provided by the invention, ammonium metavanadate is adopted as a reactant, an alkaline solvent system of the organic matter in water/absolute ethyl alcohol is used, thus the preparation method is environment-friendly, has simple preparation process and utilizes simple equipment, and the obtained NaV2O5 crystal material with L shape can be used for research on nano optical devices.
Description
Technical field
The present invention relates to a kind of right angle pattern NaV
2O
5The preparation method of crystalline material belongs to field of inorganic material preparing technology.
Background technology
There is various ways in inorganic, metal oxide at occurring in nature, and chemist wishes to obtain having the compound of different-shape, in order to expand its Application Areas synthetic various when having difform inorganic oxide always.
At present in the material of report, has diversity most based on its pattern of inorganic materials of zinc oxide.Most synthetic materials can be found similar pattern at occurring in nature, as nanotube, nanometer flower, nano wire etc.Have report to describe the iron oxide nano material of a kind of V of having font and Y font recently, this material is that the dehydration by ferrous hydroxide obtains.About 108 ° of its V font angle (CrystEngComm, 2010,12,1842-1849).But right angle pattern transition metal oxide material is not also reported.
Purpose of the present invention is to provide a kind of making about NaV
2O
5Metal oxide right angle pattern crystalline material method.Although at present to some report of crystal of this class material,, its crystal grain is little and how to exist with the nanometer rod form.We adopt a kind of simple solvent thermal synthetic route, and preparation has the NaV of right angle L type pattern in certain density alkaline solution
2O
5Crystalline material.
Summary of the invention
The object of the present invention is to provide a kind of metal oxide materials with right angle crystal morphology and preparation method thereof, can remedy the deficiency of existing crystal morphology.Synthesis device of the present invention is simple, and is easy to operate, and condition is loose, the energy is saved in less contamination, and raw material is simple and easy to, and is with low cost, and output is big, and crystalline size is controlled.
In order to achieve the above object, the present invention adopts ammonium meta-vanadate to prepare under the certain basic solution condition of organism at water/dehydrated alcohol.Ammonium meta-vanadate/organic mixed solution is aging at a certain temperature, prepares the NaV with right angle crystal morphology
2O
5Experimental technique obtains to have the right angle NaV of different size by regulating alkali and organic ratio and digestion time
2O
5
Technical scheme of the present invention is:
A kind of right angle pattern NaV
2O
5The preparation method of crystalline material may further comprise the steps:
A), the aromatic acid organism is water-soluble, and every mole of aromatic acid adds the 2-6 kg water, adds sodium hydroxide solution under stirring at normal temperature, adds solvent again, and stirring at normal temperature 40～60 minutes gets a uniform mixture;
Its material proportion is mol ratio aromatic acid organism: sodium hydroxide=1: 3.5, and every mole of aromatic acid organism adds 2.5～5 kilograms of solvents;
B), in mixture, add ammonium meta-vanadate, obtain the yellow transparent mixed solution, stir after three hours, mixture is changed over to have in the teflon-lined stainless steel cauldron, put into 150-200 ℃ aging 2-60 days of thermostatic drying chamber;
The organic mol ratio of described ammonium meta-vanadate and aromatic acid is ammonium meta-vanadate: aromatic acid organism=1～4: 1.
C), mixture takes out and filters, and 40-60 ℃ of thermostatic drying chamber inner drying obtains L type right angle NaV at last
2O
5Crystalline material.
Described aromatic acid organism is specially terephthalic acid, phthalic acid, trimesic acid, Pyromellitic Acid or their acid anhydrides.
The concentration of described sodium hydroxide solution is 2mol/l.
Described solvent is water, dehydrated alcohol or ethanolic soln.
Quality when described solvent is ethanolic soln is than water: ethanol=1: 1.
The synthetic black crystals that obtains is NaV
2O
5Material can obtain different big or small L shaped right angle NaV under different experimental conditions
2O
5Crystalline material.
Beneficial effect of the present invention is:
1. adopting ammonium meta-vanadate is reactant, uses organism in the basic solvent system of water/dehydrated alcohol, environmentally friendly.
2. can pass through to regulate the consumption of differential responses thing/organism ratio and change reaction solvent water, and the crystal growth time obtains to have the NaV of difference size
2O
5Crystalline material.
3. temperature of reaction kettle is lower, can control between 150-200 ℃.
4. preparation technology and equipment are simple, controlled NaV
2O
5The L shaped shape of crystalline material.
NaV
2O
5Crystal has optical property, the L shaped NaV that the present invention relates to
2O
5Crystal can be used for the research of nanocomposite optical device.
Description of drawings:
The x-ray diffraction pattern of the product that Fig. 1 obtains for the embodiment of the invention 1;
The low resolution transmission microscopy picture of (a) right angle crystal of Fig. 2 embodiment of the invention 1 product is the diffraction picture of right angle crystal both direction (b) and (c), (d) is the diffraction picture at crystal twin crystal boundary place, right angle.
Fig. 3 is the scanning electron microscope picture of the embodiment of the invention 1 product right angle crystal.
Fig. 4 is the opticmicroscope picture of the right angle crystal of the embodiment of the invention 2 products.
Fig. 5 is the opticmicroscope picture of the right angle crystal of the embodiment of the invention 3 products.
Embodiment
Embodiment 1: 0.210g (0.001mol) organism trimesic acid is dissolved in 5g (0.28mol) water, stir under the normal temperature and add 1.75ml NaOH solution (concentration is 2mol/l) after 5 minutes, continued stir about 15 minutes under the normal temperature, add the solvent of being formed by 2.5g water (0.14mol) and 2.5g (0.055mol) dehydrated alcohol then, obtain water white solution, at last to mixed solution and dripping 0.2339g (0.002mol) NH
4VO
3, the solution of this moment is the milk yellow muddiness, stirs after 40 minutes, and recording mixture pH is 7.5-8.0, and (mol ratio of mixture is NH
4VO
3: trimesic acid: NaOH=2: 1: 3.5; The quality of every mole of corresponding solvent of trimesic acid is 5 kilograms, water in the solvent: the mass ratio of ethanol=1.Mixture changed over to have in the teflon-lined stainless steel cauldron, put into 180 ℃ aging two days of thermostatic drying chamber, mixture is taken out filter two days later, 60 ℃ of thermostatic drying chamber inner dryings obtain L N-type waferN material at last.Fig. 1 XRD show sample is NaV
2O
5(JCPDS#70-08770, P2
1Mn (31), a=1.132nm, b=0.360nm, c=0.480nm).Crystalline diffraction such as Fig. 2, Fig. 2 a is the low transmission microscopy photo of differentiating, exist with 90 ° of angle forms between the right angle area of demonstration crystal, carry out selected diffraction (Fig. 2 b at two square edges respectively, c) show, two square edges are single crystal structure, and the square edge infall is carried out selected diffraction (Fig. 2 d), can see the twin diffraction structure that diffracting spectrum exists with two square edge stacked systems.Crystal morphology such as scanning electron microscope Fig. 3, sample mainly exist with L type appearance, reach about about 500um along the length of two square edges.
Embodiment 2: 0.210g (0.001mol) organism trimesic acid is dissolved in 5g (0.28mol) water, stir under the normal temperature and add 1.75ml NaOH solution (2mol/l) after 5 minutes, continued stir about 15 minutes under the normal temperature, add the solvent of being formed by 2.5g (0.14mol) water and 2.5g (0.055mol) dehydrated alcohol then, obtain water white solution, at last to mixed solution and dripping 0.117g (0.001mol) NH
4VO
3, the solution of this moment is the milk yellow muddiness, stirs after 60 minutes, and the pH of survey is 7.5-8.0, and (mol ratio of mixture is NH
4VO
3: trimesic acid: NaOH=1: 1: 3.5; The quality of every mole of corresponding solvent of trimesic acid is 10 kilograms, water in the solvent: the mass ratio of ethanol=1.Mixture changed over to have in the teflon-lined stainless steel cauldron, put into 180 ℃ thermostatic drying chamber internal reaction one month, then sample is taken out and filter, 40 ℃ of thermostatic drying chamber inner dryings, obtain rectangular-shaped monocrystalline at last, opticmicroscope picture (Fig. 4) shows that two square edges exist with 90 ° of angle forms, reaches about 500um, the about 50um of width along the length of two square edges.
Embodiment 3: 0.210g (0.001mol) organism trimesic acid is dissolved in 2.5g (0.14mol) water, stir under the normal temperature and add 1.75ml NaOH solution (2mol/l) after 5 minutes, continued stir about 15 minutes under the normal temperature, add the solvent of being formed by 2.5g (0.055mol) ethanol solution then, obtain water white solution, in mixing solutions, add 0.4679g (0.004mol) NH at last
4VO
3, obtain yellow muddy liquid, stirring and recording pH after 40 minutes is 7.0-7.2, the mol ratio of mixture is NH
4VO
3: trimesic acid: NaOH=4: 1: 3.5; The quality of every mole of corresponding solvent of trimesic acid is
2.5 KilogramMixture changed over to have in the teflon-lined stainless steel cauldron, put into 180 ℃ thermostatic drying chamber internal reaction 7 days, sample is taken out filter then, 40 ℃ of thermostatic drying chamber inner dryings obtain rectangular-shaped monocrystalline at last.Opticmicroscope picture (Fig. 5) shows that two square edges exist with 90 ° of angle forms, reaches about about 50um along the length of two square edges.
Embodiment 4: other experimental procedure only changes aging temperature with embodiment 1, and reaction mixture is put into 160 ℃ thermostatic drying chamber internal reaction 15 days, obtains right angle NaV
2O
5Crystal grain.
Embodiment 5: other experimental procedure is with embodiment 1, and only changing the organism trimesic acid is the organism phthalic acid, and the mol ratio 2 of ammonium meta-vanadate and phthalic acid obtains right angle NaV
2O
5Crystal grain.
Embodiment 6: other experimental procedure is with embodiment 1, and only changing the organism trimesic acid is the organism pyromellitic dianhydride, and the mol ratio 2 of ammonium meta-vanadate and pyromellitic dianhydride obtains right angle NaV
2O
5Crystal grain.
Embodiment 7: other experimental procedure is with embodiment 2, and only changing the organism trimesic acid is the organism phthalic acid, and the mol ratio 1 of ammonium meta-vanadate and organism phthalic acid obtains right angle NaV
2O
5Crystal grain.
Embodiment 8: other experimental procedure is with embodiment 3, and only changing the organism trimesic acid is pyromellitic dianhydride, the mol ratio 4 of ammonium meta-vanadate and pyromellitic dianhydride, the right angle NaV that obtains
2O
5Crystal grain.
From top embodiment as can be seen, the present invention uses the organism trimesic acid, and the mol ratio of ammonium meta-vanadate and trimesic acid is that 1 o'clock right angle sample throughput is the highest.Except right angle pattern crystal, also have other pattern particle simultaneously when using phthalic acid, trimesic acid, Pyromellitic Acid or acid anhydrides, product purity reduces.Temperature of reaction can be carried out at 150～200 ℃ among the present invention, and is best with the sample topography that 180 ℃ of reactions obtain.Compare right angle pattern NaV with current techniques
2O
5The preparation temperature of crystal is lower, and right angle crystal yardstick is controlled, the product purity height.
Claims (2)
1. right angle pattern NaV
2O
5The preparation method of crystalline material is characterized by and may further comprise the steps:
A), the aromatic acid organism is water-soluble, and every mole of aromatic acid adds the 2-6 kg water, adds sodium hydroxide solution under stirring at normal temperature, adds solvent again, and stirring at normal temperature 40 ~ 60 minutes gets a uniform mixture;
Its material proportion is mol ratio aromatic acid organism: sodium hydroxide=1:3.5, and every mole of aromatic acid organism adds 2.5～5 kilograms of solvents;
B), in mixture, add ammonium meta-vanadate, obtain the yellow transparent mixed solution, stir after three hours, mixture is changed over to have in the teflon-lined stainless steel cauldron, put into 150-200 ℃ aging 2-60 days of thermostatic drying chamber;
The organic mol ratio of described ammonium meta-vanadate and aromatic acid is ammonium meta-vanadate: aromatic acid organism=1 ~ 4:1;
C), mixture takes out and filters, and 40-60 ℃ of thermostatic drying chamber inner drying obtains right angle L type NaV at last
2O
5Crystalline material;
Described aromatic acid organism is specially terephthalic acid, phthalic acid, trimesic acid, Pyromellitic Acid or their acid anhydrides;
The concentration of described sodium hydroxide solution is 2mol/l;
Described solvent is water, dehydrated alcohol or ethanolic soln.
2. right angle pattern NaV as claimed in claim 1
2O
5The preparation method of crystalline material, the quality when it is characterized by described solvent and being ethanolic soln is than water: ethanol=1:1.
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| RU2549421C2 (en) * | 2013-09-03 | 2015-04-27 | Федеральное государственное бюджетное учреждение науки Институт химии твердого тела Уральского отделения Российской академии наук | Method of obtaining nanoneedles of sodium vanadium oxide bronze |
| CN106335924B (en) * | 2016-08-12 | 2017-12-05 | 武汉理工大学 | A kind of NaV2O5Preparation method |
| CN108163891B (en) * | 2018-02-06 | 2020-09-22 | 陕西科技大学 | Three-dimensional self-assembly NaV2O5Micron powder and preparation method and application thereof |
| CN108423711B (en) * | 2018-02-06 | 2019-12-20 | 陕西科技大学 | Tetragonal phase NaV2O5·H2O nano flaky powder and preparation method and application thereof |
| CN110643973B (en) * | 2019-11-13 | 2021-11-23 | 西安近代化学研究所 | NaV2O5Preparation method of crystal film |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100347087C (en) * | 2006-06-22 | 2007-11-07 | 同济大学 | Method for preparing Nano/micro crystal of rare earth vanadate from oxide as precursor body under low temperature |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100347087C (en) * | 2006-06-22 | 2007-11-07 | 同济大学 | Method for preparing Nano/micro crystal of rare earth vanadate from oxide as precursor body under low temperature |
Non-Patent Citations (4)
| Title |
|---|
| Fang Hu et al..Synthesis and characterizations of highly crystallized α’-NaV2O5 needles prepared by a hydrothermal process.《Journal of Alloys and Compounds》.2009,第479卷全文. * |
| Hu Fang et al..Physical and Electrochemical Characterization of Hydrothermal Prepared α′-NaV2O5 Crystals.《Chem. Res. Chinese Universities》.2010,第26卷全文. * |
| L. Bouhedja et al..Lithium intercalation in α’-NayV2O5 Synthesized via the Hydrothermal Route.《Ionics》.1998,第4卷第228页第2节实验部分. |
| Lithium intercalation in α’-NayV2O5 Synthesized via the Hydrothermal Route;L. Bouhedja et al.;《Ionics》;19981231;第4卷;第228页第2节实验部分 * |
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