CN101413141A - Method for growing ZnO nano-wire array on flexible substrate - Google Patents
Method for growing ZnO nano-wire array on flexible substrate Download PDFInfo
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- CN101413141A CN101413141A CNA2008101221133A CN200810122113A CN101413141A CN 101413141 A CN101413141 A CN 101413141A CN A2008101221133 A CNA2008101221133 A CN A2008101221133A CN 200810122113 A CN200810122113 A CN 200810122113A CN 101413141 A CN101413141 A CN 101413141A
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Abstract
The invention discloses a method for growing a ZnO nanometer wire array on a flexible substrate, which comprises the following steps: putting the washed flexible substrate into a growth chamber of a pulse laser deposition device, using ZnO ceramic as a target material, introducing O2 into the growth chamber, controlling the pressure to between 0.01 and 2 Pa, and depositing a ZnO seed crystal layer through pulse laser on the flexible substrate at room temperature; and respectively preparing a zinc nitrate aqueous solution the concentration of which is between 0.01 and 0.1 mol per liter and a hexamethylenetetramine aqueous solution, mixing the two aqueous solutions according the volume ratio of 1 to 1, then immerging the flexible substrate deposited with the ZnO seed crystal layer into the mixed solution, taking out the flexible substrate after reacting for 1 to 12 hours at a temperature of between 70 and 100 DEG C, rinsing the flexible substrate by using deionized water, and drying the flexible substrate. Devices used in the method is simple and is easy to operate, the prepared ZnO nanometer wire is good in array, has even thickness and low cost, and is suitable for mass production.
Description
Technical field
The present invention relates to the growth method of ZnO nano-wire array, especially the method for growing ZnO nano-wire array on flexible substrate.
Background technology
ZnO is a kind of wide bandgap compound semiconductor material, energy gap under the room temperature is 3.37eV, exciton bind energy is up to 60meV, its exciton can be under room temperature and above temperature stable existence, be the ideal material of preparation semiconductor laser (LDs), photodiode (LEDs).The material that the micro nano structure that ZnO still finds now is the abundantest, the nanostructure of ZnO is having good using value aspect preparation nano photoelectronic devices and the nano electron device, in addition, the nanostructure of ZnO can also emission on the scene, field such as medical treatment, bio-sensing is applied.
Polyethylene terephthalate (PET) is a topmost kind in the thermoplastic polyester, it is good to have anti-creep, fatigue resistance, rub resistance and dimensional stability, wears away little and the hardness height, has toughness maximum in the thermoplastics, characteristics such as electrical insulation capability is good, and temperature influence is little.The ZnO nano-wire array of growing on PET combines the toughness of flexible substrate and the advantage of ZnO nano-wire array electroconductibility, and substrate and ZnO nano wire make it at the touch-screen industrial circle good prospects for application be arranged in conjunction with closely.With the synthetic glass of PET replacement resistive touch screen, ZnO nano wire film replaces ito thin film, has solved touch-screen working face and conductive coating in conjunction with untight problem, and as the electrode point of contact sensitivity has been improved with nano-wire array greatly.
At present, the preparation method of zinc oxide nanowire (rod) mainly contains: metal organic vapor growth (MOVPE), chemical Vapor deposition process (CVD), pulsed laser deposition (PLD), electrochemical vapour deposition (EVD), template and hydrothermal method or the like, but all be in the research exploratory stage, can't form scale production.Need expensive plant and instrument and harsh processing condition as methods such as MOVPE, CVD, PLD, hydrothermal methods simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of equipment, technology is simple, cost is low, easy-operating method at growing ZnO nano-wire array on flexible substrate.
Method at growing ZnO nano-wire array on flexible substrate of the present invention may further comprise the steps:
1) configuration concentration is the zinc nitrate aqueous solution of 0.01～0.1mol/L and the hexamethylenetetramine aqueous solution that concentration is 0.01～0.1mol/L respectively;
2) washed flexible substrate being put into pulsed laser deposition device growth room, is target with the ZnO pottery, and the distance between target and the substrate remains 4～6cm, and growth room's vacuum tightness is evacuated to 10 at least
-3Pa, the growth room feeds O
2Gas, control pressure is 0.01～2Pa, under the room temperature on flexible substrate pulsed laser deposition ZnO inculating crystal layer;
3) with zinc nitrate aqueous solution and the 1:1 mixing by volume of the hexamethylenetetramine aqueous solution, the flexible substrate with the above-mentioned ZnO of depositing inculating crystal layer is immersed in the mixing solutions again, takes out behind reaction 1～12h down at 70～100 ℃, uses rinsed with deionized water, and oven dry gets final product.
Above-mentioned flexible substrate can be polyethylene terephthalate (PET), polyimide (PI) polybenzimidazole (PBD), polybenzoxazoles (PBO), polyethylene (PE), polypropylene (PP), polystyrene (PS) or poly-to (ethylene naphthalate) (PEN).
The length of the ZnO nano wire of growth can be controlled by the time that adjusting is immersed in the mixing solutions.
Usually, the laser power of pulsed laser deposition is 150～300mJ, laser repetition rate 3Hz.
Beneficial effect of the present invention is:
1) the inventive method equipment used is simple, and is easy to operate, and cost is low, is suitable for scale operation.
2) Zhi Bei ZnO nano-wire arrayization is good, and even thickness combines the advantage of flexible substrate and ZnO nano-wire array, has broad application prospects in the touch-screen field.
Description of drawings
Fig. 1 is the SEM figure of ZnO nano-wire array.
Embodiment
The present invention is further illustrated below in conjunction with example.
Embodiment 1
1) configuration concentration is the zinc nitrate aqueous solution of 0.05mol/L and the hexamethylenetetramine aqueous solution that concentration is 0.05mol/L respectively;
The PET substrate that 2) will clean is put into pulsed laser deposition device growth room, is target with the ZnO pottery, and the distance between target and the substrate remains 4.5cm, and growth room's vacuum tightness is evacuated to 10 at least
-3Pa, the growth room feeds O
2Gas, control pressure is 0.03Pa, and laser power is 210mJ, and laser repetition rate 3Hz deposits 2min under the room temperature on the PET substrate, obtain the ZnO inculating crystal layer;
3) with zinc nitrate aqueous solution and the 1:1 mixing by volume of the hexamethylenetetramine aqueous solution, flexible substrate with the above-mentioned ZnO of depositing inculating crystal layer is immersed in the mixing solutions again, takes out behind the reaction 6h down at 90 ℃, with deionized water rinsing repeatedly, oven dry makes the ZnO nano-wire array.
The ZnO nano-wire array as shown in Figure 1, mean diameter is 0.8 μ m, the length of ZnO nano wire is 600nm.
Embodiment 2
1) configuration concentration is the zinc nitrate aqueous solution of 0.01mol/L and the hexamethylenetetramine aqueous solution that concentration is 0.01mol/L respectively;
The PET substrate that 2) will clean is put into pulsed laser deposition device growth room, is target with the ZnO pottery, and the distance between target and the substrate remains 6cm, and growth room's vacuum tightness is evacuated to 10 at least
-3Pa, the growth room feeds O
2Gas, control pressure is 0.02Pa, and laser power is 150mJ, and laser repetition rate 3Hz deposits 5min under the room temperature on the PET substrate, obtain the ZnO inculating crystal layer;
3) with zinc nitrate aqueous solution and the 1:1 mixing by volume of the hexamethylenetetramine aqueous solution, flexible substrate with the above-mentioned ZnO of depositing inculating crystal layer is immersed in the mixing solutions again, take out behind the reaction 1h down at 100 ℃, with deionized water rinsing repeatedly, oven dry makes even thickness, length is the ZnO nano-wire array of 200nm.
Embodiment 3
1) configuration concentration is the zinc nitrate aqueous solution of 0.1mol/L and the hexamethylenetetramine aqueous solution that concentration is 0.1mol/L respectively;
The PI substrate that 2) will clean is put into pulsed laser deposition device growth room, is target with the ZnO pottery, and the distance between target and the substrate remains 6cm, and growth room's vacuum tightness is evacuated to 10 at least
-3Pa, the growth room feeds O
2Gas, control pressure is 0.2Pa, and laser power is 300mJ, and laser repetition rate 3Hz deposits 2min under the room temperature on the PI substrate, obtain the ZnO inculating crystal layer;
3) volume ratio of zinc nitrate aqueous solution and the hexamethylenetetramine aqueous solution being pressed 1:1 is mixed, PI substrate with the above-mentioned ZnO of depositing inculating crystal layer is immersed in the mixing solutions again, take out behind the reaction 12h down at 70 ℃, with deionized water rinsing repeatedly, oven dry makes even thickness, length is the ZnO nano-wire array of 1 μ m.
Claims (3)
- The method of 1 growing ZnO nano-wire array on flexible substrate may further comprise the steps:1) configuration concentration is the zinc nitrate aqueous solution of 0.01～0.1mol/L and the hexamethylenetetramine aqueous solution that concentration is 0.01～0.1mol/L respectively;2) washed flexible substrate being put into pulsed laser deposition device growth room, is target with the ZnO pottery, and the distance between target and the substrate remains 4～6cm, and growth room's vacuum tightness is evacuated to 10 at least -3Pa, the growth room feeds O 2Gas, control pressure is 0.01～2Pa, under the room temperature on flexible substrate pulsed laser deposition ZnO inculating crystal layer;3) with zinc nitrate aqueous solution and the 1:1 mixing by volume of the hexamethylenetetramine aqueous solution, the flexible substrate with the above-mentioned ZnO of depositing inculating crystal layer is immersed in the mixing solutions again, takes out behind reaction 1～12h down at 70～100 ℃, uses rinsed with deionized water, and oven dry gets final product.
- 2. the method for growing ZnO nano-wire array on flexible substrate according to claim 1, it is characterized in that said flexible substrate is polyethylene terephthalate, polyimide, polybenzimidazole, polybenzoxazoles, polyethylene, polypropylene, polystyrene or poly-to (ethylene naphthalate).
- 3. the method for growing ZnO nano-wire array on flexible substrate according to claim 1, the laser power that it is characterized in that pulsed laser deposition is 150～300mJ, laser repetition rate 3Hz.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719886A (en) * | 2012-06-20 | 2012-10-10 | 大连民族学院 | Method for growing large-area zinc oxide micron wall |
| CN103060910A (en) * | 2012-12-31 | 2013-04-24 | 苏州汶颢芯片科技有限公司 | Method for electrochemically preparing sea-urchin-shaped ZnO nanowire arrays on organic flexible material |
| CN103526165A (en) * | 2013-10-21 | 2014-01-22 | 京东方科技集团股份有限公司 | Transparent conducting thin film as well as preparation method thereof, display base plate and display device |
| CN104465112A (en) * | 2014-12-11 | 2015-03-25 | 浙江大学 | Self-driven ZnO-based ultraviolet detector based on flexible substrates and preparation method thereof |
| WO2016030746A1 (en) | 2014-08-26 | 2016-03-03 | King Abdullah University Of Science And Technology | Synthesis of vertically aligned metal oxide nanostructures |
| CN105543960A (en) * | 2015-12-16 | 2016-05-04 | 天津大学 | Method for preparing monocrystalline porous cobalt(II) oxide nanorod array |
| CN111132926A (en) * | 2017-05-01 | 2020-05-08 | 莫纳什大学 | Elastic conductor based on vertical nano-wire |
| CN112158875A (en) * | 2020-10-09 | 2021-01-01 | 南京信息工程大学 | Preparation method of isolated ZnO micron rod |
-
2008
- 2008-10-28 CN CN2008101221133A patent/CN101413141B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719886A (en) * | 2012-06-20 | 2012-10-10 | 大连民族学院 | Method for growing large-area zinc oxide micron wall |
| CN102719886B (en) * | 2012-06-20 | 2016-02-17 | 大连民族学院 | A kind of method of large area deposition zinc oxide micrometer wall |
| CN103060910A (en) * | 2012-12-31 | 2013-04-24 | 苏州汶颢芯片科技有限公司 | Method for electrochemically preparing sea-urchin-shaped ZnO nanowire arrays on organic flexible material |
| CN103526165A (en) * | 2013-10-21 | 2014-01-22 | 京东方科技集团股份有限公司 | Transparent conducting thin film as well as preparation method thereof, display base plate and display device |
| WO2015058551A1 (en) * | 2013-10-21 | 2015-04-30 | 京东方科技集团股份有限公司 | Transparent conductive film and preparation method, display substrate and display device therefor |
| WO2016030746A1 (en) | 2014-08-26 | 2016-03-03 | King Abdullah University Of Science And Technology | Synthesis of vertically aligned metal oxide nanostructures |
| CN104465112A (en) * | 2014-12-11 | 2015-03-25 | 浙江大学 | Self-driven ZnO-based ultraviolet detector based on flexible substrates and preparation method thereof |
| CN105543960A (en) * | 2015-12-16 | 2016-05-04 | 天津大学 | Method for preparing monocrystalline porous cobalt(II) oxide nanorod array |
| CN111132926A (en) * | 2017-05-01 | 2020-05-08 | 莫纳什大学 | Elastic conductor based on vertical nano-wire |
| CN112158875A (en) * | 2020-10-09 | 2021-01-01 | 南京信息工程大学 | Preparation method of isolated ZnO micron rod |
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