CN101891250A - Phase-change material compounded with strip VO2 nanoflower structure on silicon substrate and preparation method thereof - Google Patents

Phase-change material compounded with strip VO2 nanoflower structure on silicon substrate and preparation method thereof Download PDF

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Publication number
CN101891250A
CN101891250A CN 201010212063 CN201010212063A CN101891250A CN 101891250 A CN101891250 A CN 101891250A CN 201010212063 CN201010212063 CN 201010212063 CN 201010212063 A CN201010212063 A CN 201010212063A CN 101891250 A CN101891250 A CN 101891250A
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silicon substrate
strip
change material
preparation
phase
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蒋雯陶
郁可
倪娟
朱自强
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East China Normal University
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East China Normal University
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Abstract

The invention discloses a phase-change material compounded with a strip VO2 nanoflower structure on a silicon substrate and a preparation method thereof. The material comprises the silicon substrate and a VO2 crystal which grows on the silicon substrate; and the VO2 crystal grows in a direction vertical to the silicon substrate, has a strip nanoflower structure, and is directionally generated by nanobelts. The preparation method comprises the following steps of: adding ammonium metavanadate into the aqueous solution of oxalic acid, impregnating a silicon wafer in the aqueous solution, reacting at the temperature of between 150 and 180 DEG C under the sealed condition for 24 to 36 hours, and naturally cooling to the temperature of between 18 and 25 DEG C to prepare the phase-change material. The material serving as the cathode material of a Li cell has the advantages of high charging and discharging performance and cyclic voltammetry performance, stable material charging and discharging, and reusability. The phase-change material compounded with the strip VO2 nanoflower structure on the silicon substrate and the preparation method have the advantages of low cost, simple growth condition, high repeatability, safety and the like, and are suitable for large-scale industrialized production.

Description

Compounded with strip VO on silicon substrate 2The phase change material of nanometer flower structure and preparation method
Technical field
The present invention relates to photoelectron material, semiconductor material and device technology field, specifically a kind of on silicon substrate compounded with strip VO 2Phase change material of nanometer flower structure and preparation method thereof.
Background technology
VO 2Be a kind of thermal induced phase transition compound, under the monocrystalline state, near about 68 ℃ of temperature, can present tangible metal-semiconductor phase transformation characteristics.When temperature is lower than 68 ℃, VO 2Be in the semi-conductor attitude, be monoclinic structure; When temperature is higher than 68 ℃, VO 2Change metallic state into, have cubic rutile structure, and phase transformation is very fast.
Be accompanied by the generation of phase transformation, its many physical propertiess are all undergone mutation as refractive index n, reflectivity R and resistivity etc., and wherein the variation amplitude of resistivity especially can be up to 10 4Magnitude is utilized its these characteristics, VO 2Be widely used in electric switch and light shutter device.As functional materials, it has wide application prospects in fields such as temperature sensing, optical storage, variable reflectivity mirror, lasing safety and smart window.
Recently, people utilize the whole bag of tricks (solution method, sol-gel method, thermal evaporation etc.) to prepare various VO 2Film and one dimension VO 2Nanostructure, for example, nano wire, nano belt, nanometer rod etc., and the phase-change characteristic of these nanostructures studied.The employing Hydrothermal Preparation VO that on Nano Letters, reports as Mai Liqiang etc. 2Nano wire, the employing Hydrothermal Preparation VO that Guicun Li etc. reports on Inorganic Chemistry 2Nano belt.
But, above-mentioned nano wire, nano belt, nanometer rod etc. are one dimension VO 2Therefore nanostructure, when reality is used, can't satisfy the needs in relevant field, also is difficult to be applied to large-scale industrial production, and severe reaction conditions, and production cost is high.
Summary of the invention
One of purpose of the present invention be to provide a kind of on silicon substrate compounded with strip VO 2The phase change material of nanometer flower structure is to overcome the above-mentioned defective that prior art exists.
Second purpose of the present invention is to provide the preparation method of above-mentioned materials, so that suitability for industrialized production.
The object of the present invention is achieved like this:
A kind of on silicon substrate compounded with strip VO 2The phase change material of nanometer flower structure comprises silicon substrate and the VO that is grown on the substrate 2Crystal, described VO 2The crystal edge is perpendicular to the growth of silicon substrate direction, and described VO 2Crystal is banded nanometer flower structure, generates by nano belt is directed, and the diameter of nanometer flower structure is 10~18 μ m.
Described banded VO 2Nanometer flower structure refers to, at described VO 2The crystalline surface has the nano belt of outside stretching, extension, and the width of nano belt is 100~700nm.
Described on silicon substrate compounded with strip VO 2The preparation method of the phase change material of nanometer flower structure may further comprise the steps:
With ammonium meta-vanadate (NH 4VO 3) adding oxalic acid (C 2H 2O 4) aqueous solution, then silicon chip be impregnated in the described aqueous solution, under air-tight state, 150~180 ℃ the reaction 24~36 hours, naturally cool to 18~25 ℃, obtain described on silicon substrate compounded with strip VO 2The phase change material of nanometer flower structure.
Described oxalic acid (C 2H 2O 4) concentration of the aqueous solution is 0.0075~0.0125g/ml.
The weight ratio of ammonium meta-vanadate and oxalic acid is: ammonium meta-vanadate: oxalic acid=1: 0.4~1: 1.1.
The present invention compared with prior art has novel structure, and preparation process is simple, and production cost is low, and repeatable advantages of higher can be suitable for the development of integrated nanometer opto-electronic device in conjunction with present sophisticated semiconductor silicon integrated circuit technology.The material of the present invention's preparation has good charge-discharge performance and cyclic voltammetric performance as the cathode material of Li battery, and material discharges and recharges stable, and is reusable.The present invention has advantages such as cost is low, and growth conditions is simple, and repeatability is high, and is safe, is suitable for large-scale industrial production.
Description of drawings
Fig. 1 is the X-ray diffractogram of the embodiment of the invention 1 gained material
Fig. 2 is the SEM figure of the embodiment of the invention 1 gained material
Fig. 3 is the SEM figure of the embodiment of the invention 1 gained material magnification
Fig. 4 is the single banded VO of the embodiment of the invention 1 gained material 2The SEM figure of nanometer flower structure
Fig. 5 is the single banded VO of the embodiment of the invention 2 gained materials 2The SEM figure of nanometer flower structure
Fig. 6 is the single banded VO of the embodiment of the invention 3 gained materials 2The SEM figure of nanometer flower structure
Embodiment
Embodiment 1
(a), with 0.38g oxalic acid (C 2H 2O 4) powder is dissolved in the 40ml water, uses magnetic stirrer, powder all after the dissolving, adds 0.4g ammonium meta-vanadate (NH in solution 4VO 3) powder, continue to stir, form safran solution.
(b) earlier the silicon chip that cleans up is put into autoclave, more above-mentioned solution is poured into the autoclave of 50ml, behind the autoclave good seal, put into air dry oven, under 160 ℃ of temperature, keep reaction 24 hours, be cooled to room temperature naturally, promptly make compounded with strip VO on silicon chip 2The phase change material of nanometer flower structure.
Described VO 2Crystal is banded VO 2Nanometer flower structure generates banded VO by nano belt is directed 2The nanometer flower structure diameter is 11um, and described nano belt width is 100nm.
Banded VO 2The X-ray diffractogram of nanometer flower structure is seen Fig. 1, banded VO 2The SEM figure of nanometer flower structure sees Fig. 2, banded VO 2The SEM figure of the magnification of nanometer flower structure sees Fig. 3, one banded VO 2The SEM figure of nanometer flower structure sees Fig. 4.
Embodiment 2
(a) with 0.4g oxalic acid (C 2H 2O 4) powder is dissolved in the 40ml water, uses magnetic stirrer, powder all after the dissolving, adds 0.3g ammonium meta-vanadate (NH in solution 4VO 3) powder, continue to stir, form safran solution.
(b) the banded VO of growth on silicon chip 2Nanometer flower structure: earlier the silicon chip that cleans up is put into autoclave, again above-mentioned solution is poured into the autoclave of 50ml, will be put into air dry oven behind the autoclave good seal, under 160 ℃ of temperature, keep reaction 24 hours, naturally be cooled to room temperature, promptly make compounded with strip VO on silicon chip 2The phase change material of nanometer flower structure.
Described VO 2Crystal is banded VO 2Nanometer flower structure generates banded VO by nano belt is directed 2The diameter of nanometer flower structure is 12 μ m, and the width of described nano belt is 200nm.
Its X-ray diffractogram is similar substantially to embodiment 1, single banded VO 2The SEM figure of nanometer flower structure sees Fig. 5.
Embodiment 3
(a) with 0.45 oxalic acid (C 2H 2O 4) powder is dissolved in the 40ml water, uses magnetic stirrer, powder all after the dissolving, adds 0.5g ammonium meta-vanadate (NH in solution 4VO 3) powder, continue to stir, form pale yellow solution.
(b) the banded VO of growth on silicon chip 2Nanometer flower structure: earlier the silicon chip that cleans up is put into autoclave, again above-mentioned solution is poured into the autoclave of 50ml, will be put into air dry oven behind the autoclave good seal, under 180 ℃ of temperature, keep reaction 36 hours, naturally be cooled to room temperature, promptly make compounded with strip VO on silicon chip 2The phase change material of nanometer flower structure.
Described VO 2Crystal is banded VO 2Nanometer flower structure generates banded VO by nano belt is directed 2The diameter of nanometer flower structure is 18 μ m, the width 700nm of described nano belt.
Its X-ray diffractogram is similar substantially to embodiment 1, banded VO 2The SEM figure of nanometer flower structure sees Fig. 6.

Claims (3)

1. compounded with strip VO on silicon substrate 2The phase change material of nanometer flower structure is characterized in that this material comprises silicon substrate and the VO that is grown on the described substrate 2Crystal, its VO 2Crystal along perpendicular to silicon substrate direction growth, be banded nanometer flower structure and by the directed generation of nano belt.
2. phase change material according to claim 1 is characterized in that the nanometer flower diameter is 10~18 μ m; The nano belt width is 100~700nm.
3. described preparation methods of claim 1 is characterized in that this method may further comprise the steps:
Ammonium meta-vanadate is added oxalic acid aqueous solution, silicon substrate be impregnated in the described aqueous solution, under air-tight state, 150~180 ℃ were reacted 24~36 hours, naturally cooled to 18~25 ℃, obtained compounded with strip VO on silicon substrate 2The phase change material of nanometer flower structure; Wherein: the concentration of described oxalic acid aqueous solution is 0.0075~0.0125g/ml; The weight ratio of ammonium meta-vanadate and oxalic acid is: ammonium meta-vanadate: oxalic acid=1: 0.7~1: 1.1.
CN 201010212063 2010-06-25 2010-06-25 Phase-change material compounded with strip VO2 nanoflower structure on silicon substrate and preparation method thereof Pending CN101891250A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105669248A (en) * 2016-01-04 2016-06-15 北京理工大学 Vanadium dioxide thin film having regular truss network structure and preparation method thereof
CN105948121A (en) * 2016-05-04 2016-09-21 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing highly pure vanadium dioxide
CN106486158A (en) * 2016-10-20 2017-03-08 盐城工学院 Memory and method to infrared photon memory storage

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62201645A (en) * 1986-02-27 1987-09-05 Kawasaki Steel Corp Production of catalyst for producing pyromellitic acid anhydride
CN101746705A (en) * 2009-12-11 2010-06-23 华东师范大学 Phase-change material for compositing VO2 nanometer flower structure on silicon wafer and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62201645A (en) * 1986-02-27 1987-09-05 Kawasaki Steel Corp Production of catalyst for producing pyromellitic acid anhydride
CN101746705A (en) * 2009-12-11 2010-06-23 华东师范大学 Phase-change material for compositing VO2 nanometer flower structure on silicon wafer and preparation method thereof

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* Cited by examiner, † Cited by third party
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105669248A (en) * 2016-01-04 2016-06-15 北京理工大学 Vanadium dioxide thin film having regular truss network structure and preparation method thereof
CN105948121A (en) * 2016-05-04 2016-09-21 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing highly pure vanadium dioxide
CN106486158A (en) * 2016-10-20 2017-03-08 盐城工学院 Memory and method to infrared photon memory storage
CN106486158B (en) * 2016-10-20 2020-09-25 盐城工学院 Memory and method for infrared photon memory storage

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