CN101172655A - Method of producing LiNbO* nanowire - Google Patents
Method of producing LiNbO* nanowire Download PDFInfo
- Publication number
- CN101172655A CN101172655A CNA2007101561855A CN200710156185A CN101172655A CN 101172655 A CN101172655 A CN 101172655A CN A2007101561855 A CNA2007101561855 A CN A2007101561855A CN 200710156185 A CN200710156185 A CN 200710156185A CN 101172655 A CN101172655 A CN 101172655A
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- reactor
- linbo
- preparation
- substrate
- reaction kettle
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- 239000002070 nanowire Substances 0.000 title claims description 25
- 238000000034 method Methods 0.000 title abstract description 4
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims description 26
- 229910013641 LiNbO 3 Inorganic materials 0.000 claims description 17
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- 239000010409 thin film Substances 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 238000010897 surface acoustic wave method Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910003327 LiNbO3 Inorganic materials 0.000 abstract 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 abstract 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract 2
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 10
- 239000002086 nanomaterial Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000012010 growth Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- 230000007123 defense Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method for LiNbO3 nanometer rod. The method comprises the steps as follow: LiOH.H2O, Nb2O5 and KOH are used as reactants and are arranged in a reaction kettle; a lining base is tipsily arranged inside the reaction kettle; and deionized water is added into the reaction kettle till reaching 80 percent of the volume of the reaction kettle, and then the reaction kettle is sealed and is kept with temperature range from 150 DEG C to 220 DEG C for 1 to 7 days for hydro-thermal reaction, so as to obtain LiNbO3 nanometer rod. The invention has the advantages of simple device, low cost, and easy operation. Besides, the necessary raw material is easy to get and has high reuse performance. The invention solves the problem of breaking into nanometer level from micron level of the LiNbO3 light guide and surface acoustic wave device preparation. The LiNbO3 nanometer rod prepared with the invention has more advantages in the application aspect of the light guide and surface acoustic wave device.
Description
Technical field
The present invention relates to the preparation of nano material, relate to a kind of LiNbO specifically
3The preparation method of nano wire.
Background technology
Nano wire, nano particle, because the electricity and the optical property of the excellence that quantum limitation effect had, showing tempting prospect aspect electricity, the optical device, as make diode, logical integrated circuit, photodiode, quantum dot laser, biosystem probe and various photoconverter or modulator, photochemical catalysis etc., therefore cause whole world extensive studies interest.Along with developing rapidly of mobile communcations system, more and more higher to the microminiaturization requirement of device, traditional build components and parts more and more are difficult to satisfy current needs on volume.III-V family and IV family nano wire, nano-particle material growth and device application research have obtained huge progress, for new nanometer information technology is laid a good foundation.
Aspect the preparation of nano material: unitary nano material such as carbon nanotube, silicon nanowires and metal nanometer line nano particle are studied the earliest, and its preparation and application have obtained huge achievement; Also obtaining huge progress aspect the nano material of binary compound, people successfully prepare the oxide-based nanomaterial of various III-V family's semiconductor nano materials and binary.But at multi-element compounds, particularly the nano material preparation aspect of multivariant oxide is studied in the world also in the starting stage, and this mainly is owing to the increase along with the compound composition, has increased its preparation difficulty.Although the preparation of multi-element compounds nano wire has certain degree of difficulty, present having successfully prepares BaTiO
3Report with ternary oxide nano wires such as PZT.
Lithium niobate crystals has good piezoelectricity, electric light, acousto-optic, performance such as non-linear.At military, civil area purposes is widely arranged, along with the development of photoelectric technology, LiNbO
3The application of crystal in defense technology more and more comes into one's own.LiNbO
3Research can trace back to 1949 and nineteen fifty-one to LiNbO
3The ferroelectric report of monocrystalline.Subsequently, Bell Laboratory is to LiNbO
3Crystalline structure piezoelectric effect, electrooptical property and acoustic properties etc. done extensive and deep research.Along with the appearance of optical fiber and the rise of integrated optics, LiNbO
3Crystal has obtained enough attention in the application aspect optical waveguides and the integrated optics.As surface acoustic wave (SAW) device is a kind of high-tech electronic product that integrates acoustics, electronics, piezoelectric and semiconductor planar technology that grows up in the phase at the end of the sixties in last century.The SAW device is owing to have advantages such as miniaturization, high reliability, multi-functional and high conformity, thereby obtained to use widely in the civilian and national defense industry field at opticfiber communication, TV, radar, sonar, electronic countermeasure etc.LiNbO
3Material is exactly the important materials of preparation SAW device.But the LN device also stops and uses on body monocrystalline, the thin-film material microelectronic technique, along with the development of microelectronics to Nanoelectronic Technology, LiNbO at present
3Material also will develop to the nano material preparation direction, so the research of LN nano wire has important meaning to China's Sustainable development.
The present favourable Hydrothermal Preparation LiNbO that uses
3The report of nano particle, existing investigator utilizes aluminum oxide porous template to prepare LiNbO
3Nanotube.But also do not prepare LiNbO
3Nano wire report.
Summary of the invention
The purpose of this invention is to provide a kind of LiNbO
3The preparation method of nano wire.
LiNbO of the present invention
3The preparation method of nano wire is characterized in that may further comprise the steps:
1) with LiOHH
2O, Nb
2O
5, KOH 2: 1: 7 in molar ratio～14 places reactor; And then substrate tilting is positioned in the reactor;
2) in reactor, inject deionized water to 80% of reactor volume, sealed reactor, heating is incubated 1 to 7 day down at 150 ℃～220 ℃ and carries out hydro-thermal reaction, naturally cools to room temperature;
3) take out substrate, dry down at 80 ℃.
Among the present invention, said substrate can be aluminum oxide or the top aluminum oxide that evaporates one deck nano thickness gold thin film.
The inventive method can be controlled LiNbO by strength of solution, potential of hydrogen, hydrothermal temperature and reaction times in the adjusting hydro-thermal reaction
3The growth length and the size of nano wire.
Substrate tilting is positioned over allows the nano particle that generates sink to the reactor bottom in the reactor, better on substrate, generate nano wire, avoid nano particle to sneak in the nano wire.
Beneficial effect of the present invention is:
Preparation method's equipment simple cheap of the present invention, easy handling; Desired raw material is easy to get, reuse is strong; Solved LiNbO
3Material optical waveguides, surface acoustic wave device preparation stride into problem by micron level to nanometer level, the LiNbO that makes
3Nano wire has greater advantages in optical waveguides and acoustic wave device application facet.
Description of drawings
Fig. 1 is the XRD figure of white powder;
Fig. 2 is LiNbO on the substrate
3Stereoscan photograph;
Fig. 3 is LiNbO on the substrate
3The TEM photo of nano wire.
Embodiment
Below further specify LiNbO of the present invention by example
3The preparation method of nano wire.
Embodiment 1
1) with the analytical pure LiOHH of 0.10g
2The analytical pure Nb of O, 0.30g
2O
5Analytical pure KOH (mol ratio LiOHH with 0.70g
2O: Nb
2O
5: KOH=2: 1: 10.5) add in the reactor successively.
2) prepare to have evaporated above the portion alumina substrate of one deck nano thickness gold thin film, be cut to rectangle, the long limit of orthogonal is slightly less than the interior path length of reactor.This substrate is put into reactor, make long limit level during placement, substrate just is skewed in hydrothermal reaction kettle like this.
3) in reactor, inject deionized water to 80% of reactor volume, behind the reactor good seal, be incubated 7 days down at 150 ℃ and carry out hydro-thermal reaction, naturally cool to room temperature then.
4) carefully take out substrate from reactor, 80 ℃ of dryings obtain LiNbO in loft drier
3Nano wire.
In order to detect the composition of resultant on the substrate, the white precipitate bottom the reactor is carried out following processing:
The still of falling dereaction supernatant liquid is got the reactor bottom settlings and is placed furnace pot to evaporate redundant moisture, and the white powder that obtains is placed 80 ℃ of dryings of loft drier, takes out and carries out the XRD test, and test result is seen Fig. 1.The peak of Fig. 1 is mainly by LiNbO
3, Li
3NbO
4And LiNb
3O
8Form, wherein, LiNbO
3Be topmost.Because material obtains under the same conditions on powder and the substrate, so the composition on the substrate is the same with the powder composition, so the material on the substrate also is with LiNbO
3Be main.
The stereoscan photograph of substrate is seen Fig. 2, as can be seen from the figure, and LiNbO
3Nano wire is the bandlet shape, and the nano wire top is taper.
Embodiment 2
1) with LiOHH
2O, Nb
2O
5, KOH placed reactor in 2: 1: 13 in molar ratio; And then top alumina substrate of having evaporated one deck nano thickness gold thin film tilted to be positioned in the reactor;
2) in reactor, inject deionized water to 80% of reactor volume, sealed reactor, heating is incubated 2 days down at 220 ℃ and carries out hydro-thermal reaction, naturally cools to room temperature;
3) take out substrate, dry down at 80 ℃.
Material on the substrate that this example obtains also is LiNbO
3Composition.The TEM photo of substrate is seen Fig. 3, can clearly see the LiNbO of two nearly parallel growths from figure
3Nano wire.
Embodiment 2
1) with LiOHH
2O, Nb
2O
5, KOH placed reactor in 2: 1: 7 in molar ratio; And then the alumina substrate Dou that inclines is positioned in the reactor;
2) in reactor, inject deionized water to 80% of reactor volume, sealed reactor, heating is incubated 4 days down at 180 ℃ and carries out hydro-thermal reaction, naturally cools to room temperature;
3) take out substrate, dry down at 80 ℃.
Material on the substrate that this example obtains also is LiNbO
3Nano wire.
Claims (2)
1. LiNbO
3The preparation method of nano wire is characterized in that may further comprise the steps:
1) with LiOHH
2O, Nb
2O
5, KOH 2: 1: 7 in molar ratio～14 places reactor; And then the substrate Dou that inclines is positioned in the reactor;
2) inject deionized water to 80% of reactor volume in reactor, sealed reactor is incubated 1 to 7 day down at 150 ℃～220 ℃ and carries out hydro-thermal reaction, naturally cools to room temperature;
3) take out substrate, dry down at 80 ℃.
2. by the described a kind of LiNbO of claim 1
3The preparation method of nano wire is characterized in that said substrate is aluminum oxide or the top aluminum oxide that evaporates one deck nano thickness gold thin film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710156185A CN100582016C (en) | 2007-10-23 | 2007-10-23 | Method of producing LiNbO* nanowire |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710156185A CN100582016C (en) | 2007-10-23 | 2007-10-23 | Method of producing LiNbO* nanowire |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101172655A true CN101172655A (en) | 2008-05-07 |
| CN100582016C CN100582016C (en) | 2010-01-20 |
Family
ID=39421444
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200710156185A Expired - Fee Related CN100582016C (en) | 2007-10-23 | 2007-10-23 | Method of producing LiNbO* nanowire |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100582016C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857272A (en) * | 2010-06-22 | 2010-10-13 | 浙江大学 | Preparation method for micro-nano acicular structural KNbO3 |
| CN102115168A (en) * | 2011-03-04 | 2011-07-06 | 浙江大学 | Preparation method of Li3NbO4 with nanostructure |
| CN104016408A (en) * | 2014-06-10 | 2014-09-03 | 南京航空航天大学 | Synthetic method of sodium niobate nanowire |
| CN106495219A (en) * | 2016-10-25 | 2017-03-15 | 北京工业大学 | Induced with laser prepares KNb3O8The method of nano wire |
| CN107159184A (en) * | 2017-04-27 | 2017-09-15 | 河南师范大学 | The method that hydro-thermal auxiliary prepares the lithium niobate photochemical catalyst of meso-hole structure three |
| CN110474029A (en) * | 2019-07-11 | 2019-11-19 | 江苏师范大学 | A kind of anode composite material of lithium sulfur battery and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3528765A (en) * | 1967-06-08 | 1970-09-15 | Union Carbide Corp | Lithium niobate crystals having elevated phase matching temperatures and method therefor |
-
2007
- 2007-10-23 CN CN200710156185A patent/CN100582016C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857272A (en) * | 2010-06-22 | 2010-10-13 | 浙江大学 | Preparation method for micro-nano acicular structural KNbO3 |
| CN102115168A (en) * | 2011-03-04 | 2011-07-06 | 浙江大学 | Preparation method of Li3NbO4 with nanostructure |
| CN102115168B (en) * | 2011-03-04 | 2012-05-02 | 浙江大学 | Preparation method of Li3NbO4 with nanostructure |
| CN104016408A (en) * | 2014-06-10 | 2014-09-03 | 南京航空航天大学 | Synthetic method of sodium niobate nanowire |
| CN104016408B (en) * | 2014-06-10 | 2016-08-17 | 南京航空航天大学 | A kind of synthetic method of sodium niobate nano line |
| CN106495219A (en) * | 2016-10-25 | 2017-03-15 | 北京工业大学 | Induced with laser prepares KNb3O8The method of nano wire |
| CN107159184A (en) * | 2017-04-27 | 2017-09-15 | 河南师范大学 | The method that hydro-thermal auxiliary prepares the lithium niobate photochemical catalyst of meso-hole structure three |
| CN107159184B (en) * | 2017-04-27 | 2021-05-04 | 河南师范大学 | Hydrothermal assisted preparation of mesoporous structure LiNb3O8Method for preparing photocatalyst |
| CN110474029A (en) * | 2019-07-11 | 2019-11-19 | 江苏师范大学 | A kind of anode composite material of lithium sulfur battery and preparation method thereof |
| CN110474029B (en) * | 2019-07-11 | 2022-06-10 | 江苏师范大学 | Lithium-sulfur battery positive electrode composite material and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100582016C (en) | 2010-01-20 |
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