CN104710110B - A kind of preparation method of vanadium oxide nanometer rods film layer - Google Patents
A kind of preparation method of vanadium oxide nanometer rods film layer Download PDFInfo
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- CN104710110B CN104710110B CN201510059742.6A CN201510059742A CN104710110B CN 104710110 B CN104710110 B CN 104710110B CN 201510059742 A CN201510059742 A CN 201510059742A CN 104710110 B CN104710110 B CN 104710110B
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Abstract
The invention belongs to nano material manufacturing technology field, is related to a kind of preparation method of vanadium oxide nanometer rods film layer.Characterized in that, the step of preparing is as follows：Prepare coated solution；Prepare wet glued membrane；Glued membrane is dried；Glued membrane is heat-treated.The present invention proposes a kind of preparation method of vanadium oxide nanometer rods film layer, and be capable of simple and fast directly prepares vanadium oxide nanometer rods film material on required substrate, meets demand of the electronic applications to vanadium oxide nanometer film material.
Description
Technical field
The invention belongs to nano material manufacturing technology field, is related to a kind of preparation method of vanadium oxide nanometer rods film layer.
Background technology
Vanadium oxide is a kind of intelligent inversion of phases material, under the triggering of the conditions such as thermal field, electric field or magnetic field, it may occur that gold
Category-insulator phase transition, the change of simultaneous crystal structure, resistivity, magnetic susceptibility, transmissivity and reflectivity all produce prominent
Become.These properties cause vanadium oxide to turn into a kind of infrared acquisition having wide application prospects, electrode of lithium cell, laser radiation and intelligence
Can window material.Vanadium oxide nano material is due to that with quantum size effect, the advantage such as surface-area effects and dimensional effect, can produce
Novel performance not available for raw many conventional materials.In recent years, people utilize number of ways (chemical method, molecular beam epitaxy, arteries and veins
Impulse light deposition, metal-organic chemical vapor deposition equipment etc.) prepare a variety of vanadium oxide nanostructureds, such as nanometer
(A.Tselev, J.D.Budai, the E.Strelcov, " Electromechanical such as particle, nano wire, nanobelt, nanometer rods
actuation and current-induced metastable states in suspended s ingle-crystal
l ine VO2nanoplatelets",Nano.Lett.,2011,11:3065-3073).The wherein nanometer material of Physical growth
Material is easy to film forming, is advantageous to the preparation and application of subsequent device, but has long preparation period, complex technical process, cost height etc.
Inferior position.Chemical method (conventional such as solvent-thermal method, microemulsion method, sol method) is although with yield height, be easy to doping, equipment work
Numerous advantages such as skill is simple, cost is cheap, but the product synthesized is hardly transferred in required substrate, while can not also avoid nanometer
Reunion and dispersion problem of the material in film forming procedure, this just strongly limit vanadium oxide applications to nanostructures scope.Cause
How this, directly prepare on required substrate vanadium oxide nanometer rods film material as urgent need to resolve using chemical method
Problem.
The content of the invention
The purpose of the present invention is：A kind of preparation method of vanadium oxide nanometer rods film layer is proposed, so as to simple and fast
Vanadium oxide nanometer rods film material is directly prepared on required substrate.
The technical scheme is that：A kind of preparation method of vanadium oxide nanometer rods film layer, it is characterised in that the step of preparation
It is rapid as follows：
1st, coated solution is prepared：Vanadyl acetylacetonate is dissolved in ethylene glycol monomethyl ether, ethylene glycol, alcohol or methanol solvate
In, 40 DEG C~60 DEG C are heated up to, stirs 1h~10h, the coated solution that concentration is 0.05mol/L~0.2mol/L is obtained, stands
24h~72h；
2nd, wet glued membrane is prepared：Coated solution is put into atomizer, sprayed coated solution in cleaning using spray-on process
On substrate base, wet glued membrane is formed, substrate base is silicon chip, quartz plate or slide；
3rd, glued membrane is dried：The substrate base for spraying wet glued membrane is put into heat-treatment furnace and carries out drying and processing, drying temperature
Spend for 80 DEG C~150 DEG C, heating rate is more than 10 DEG C/s, soaking time 1min~10min, makes wet glued membrane dryness finalization film forming；
4th, glued membrane is heat-treated：Dried substrate base is placed in tube furnace, nitrogen oxygen atmosphere is passed through and is annealed
Processing, the ratio of wherein nitrogen and oxygen is 10：1, annealing temperature is 500 DEG C ± 10 DEG C, annealing time 10min~120min,
Substrate base is taken out after being subsequently cooled to room temperature, you can obtains vanadium oxide nanometer rods film.
It is an advantage of the invention that：Propose a kind of preparation method of vanadium oxide nanometer rods film layer, be capable of simple and fast
Vanadium oxide nanometer rods film material is directly prepared on required substrate, meets electronic applications to vanadium oxide nanometer film material
Demand.
Brief description of the drawings
Fig. 1 is the SEM figures of the vanadium oxide nanometer rods film synthesized in the embodiment of the present invention 1
Fig. 2 is the SEM figures of the vanadium oxide nanometer rods film synthesized in the embodiment of the present invention 2
Embodiment
The present invention is described in further details below.A kind of preparation method of vanadium oxide nanometer rods film layer, its feature exist
It is as follows in, the preparation the step of：
1st, coated solution is prepared：Vanadyl acetylacetonate is dissolved in ethylene glycol monomethyl ether, ethylene glycol, alcohol or methanol solvate
In, 40 DEG C~60 DEG C are heated up to, stirs 1h~10h, the coated solution that concentration is 0.05mol/L~0.2mol/L is obtained, stands
24h~72h；
2nd, wet glued membrane is prepared：Coated solution is put into atomizer, sprayed coated solution in cleaning using spray-on process
On substrate base, wet glued membrane is formed, substrate base is silicon chip, quartz plate or slide；
3rd, glued membrane is dried：The substrate base for spraying wet glued membrane is put into heat-treatment furnace and carries out drying and processing, drying temperature
Spend for 80 DEG C~150 DEG C, heating rate is more than 10 DEG C/s, soaking time 1min~10min, makes wet glued membrane dryness finalization film forming；
4th, glued membrane is heat-treated：Dried substrate base is placed in tube furnace, nitrogen oxygen atmosphere is passed through and is annealed
Processing, the ratio of wherein nitrogen and oxygen is 10：1, annealing temperature is 500 DEG C ± 10 DEG C, annealing time 10min~120min,
Substrate base is taken out after being subsequently cooled to room temperature, you can obtains vanadium oxide nanometer rods film.
The present invention operation principle be：Reaction coated solution is prepared using the organic alkoxide of vanadium, then sprays into wet glued membrane,
During wet glued membrane dryness finalization, the presence of liquid phase source is remained using quick thermal treatment process, causes finally to grow
Nanometer rods lie low or be embedded in substrate, that is, formed wetting assisting growth.Under this growth conditions, two masters can be produced
Driving force is wanted, first, the interface interaction power of vanadium oxide and substrate, first, capillary force, both power collective effects promote dioxy
Change vanadium nanometer rods to grow up at high temperature film forming.
Embodiment 1
1st, coated solution is prepared：Vanadyl acetylacetonate is dissolved in ethylene glycol monomethyl ether, is heated up to 60 DEG C, 1h is stirred, obtains
Concentration is 0.05mol/L coated solution, stands 24h；
2nd, wet glued membrane is prepared：Coated solution is put into atomizer, sprayed coated solution in cleaning using spray-on process
On substrate base, wet glued membrane is formed, substrate base is quartz plate；
3rd, glued membrane is dried：The substrate base for spraying wet glued membrane is put into heat-treatment furnace and carries out drying and processing, drying temperature
Spend for 80 DEG C, heating rate is more than 10 DEG C/s, soaking time 10min, makes wet glued membrane dryness finalization film forming；
4th, glued membrane is heat-treated：Dried substrate base is placed in tube furnace, nitrogen oxygen atmosphere is passed through and is annealed
Processing, the ratio of wherein nitrogen and oxygen is 10：1, annealing temperature is 500 DEG C ± 10 DEG C, annealing time 10min, is then cooled down
Substrate base is taken out after to room temperature, you can obtains vanadium oxide nanometer rods film.
Fig. 1 is the SEM figures of the vanadium oxide nanometer rods film synthesized in embodiment 1.From the figure, it can be seen that prepared oxygen
Change vanadium nanometer rods quantity more and be evenly distributed, length is about 2 microns, and width is about 0.3~0.5 micron.
Embodiment 2
1st, coated solution is prepared：Vanadyl acetylacetonate is dissolved in alcohol, is heated up to 40 DEG C, stirs 10h, obtaining concentration is
0.2mol/L coated solution, stand 72h；
2nd, wet glued membrane is prepared：Coated solution is put into atomizer, sprayed coated solution in cleaning using spray-on process
On substrate base, wet glued membrane is formed, substrate base is silicon chip；
3rd, glued membrane is dried：The substrate base for spraying wet glued membrane is put into heat-treatment furnace and carries out drying and processing, drying temperature
Spend for 150 DEG C, heating rate is more than 10 DEG C/s, soaking time 1min, makes wet glued membrane dryness finalization film forming；
4th, glued membrane is heat-treated：Dried substrate base is placed in tube furnace, nitrogen oxygen atmosphere is passed through and is annealed
Processing, the ratio of wherein nitrogen and oxygen is 10：1, annealing temperature is 500 DEG C ± 10 DEG C, annealing time 120min, is then cooled down
Substrate base is taken out after to room temperature, you can obtains vanadium oxide nanometer rods film.
Fig. 2 is the SEM figures of the vanadium oxide nanometer rods film synthesized in embodiment 2.From the figure, it can be seen that prepared oxygen
Change vanadium nanometer rods quantity more and be evenly distributed, length is about 500 nanometers, and width is about 100 nanometers.
Claims (1)
1. a kind of preparation method of vanadium oxide nanometer rods film layer, it is characterised in that as follows the step of preparation：
1.1st, coated solution is prepared：Vanadyl acetylacetonate is dissolved in ethylene glycol monomethyl ether, ethylene glycol, alcohol or methanol solvate,
40 DEG C~60 DEG C are heated up to, stirs 1h~10h, the coated solution that concentration is 0.05mol/L~0.2mol/L is obtained, stands 24h
~72h；
1.2nd, wet glued membrane is prepared：Coated solution is put into atomizer, coated solution is sprayed to the lining in cleaning using spray-on process
In bottom substrate, wet glued membrane is formed, substrate base is silicon chip, quartz plate or slide；
1.3rd, glued membrane is dried：The substrate base for spraying wet glued membrane is put into heat-treatment furnace and carries out drying and processing, drying temperature
For 80 DEG C~150 DEG C, heating rate is more than 10 DEG C/s, soaking time 1min~10min, makes wet glued membrane dryness finalization film forming；
1.4th, glued membrane is heat-treated：Dried substrate base is placed in tube furnace, nitrogen oxygen atmosphere is passed through and carries out at annealing
Reason, the ratio of wherein nitrogen and oxygen is 10：1, annealing temperature is 500 DEG C ± 10 DEG C, annealing time 10min~120min, so
After be cooled to room temperature after take out substrate base, you can obtain vanadium oxide nanometer rods film.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805131A (en) * | 2010-03-18 | 2010-08-18 | 中国科学院上海硅酸盐研究所 | Low-temperature preparation method and application of vanadium dioxide film |
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| CN101805131A (en) * | 2010-03-18 | 2010-08-18 | 中国科学院上海硅酸盐研究所 | Low-temperature preparation method and application of vanadium dioxide film |
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