CN105428534B - A kind of ultraviolet photovoltaic detector with ZnO nanorod with luxuriant and rich with fragrance nano heterogeneous composite construction - Google Patents
A kind of ultraviolet photovoltaic detector with ZnO nanorod with luxuriant and rich with fragrance nano heterogeneous composite construction Download PDFInfo
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- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
- H10K30/152—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising zinc oxide, e.g. ZnO
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Abstract
A kind of ultraviolet photovoltaic detector with ZnO nanorod and luxuriant and rich with fragrance nano heterogeneous composite construction, belongs to semiconductor and nano photoelectronic devices field, more particularly to the ultraviolet photovoltaic detector of a kind of ZnO nanorod and luxuriant and rich with fragrance nano heterogeneous composite construction preparation method.The base material of the detector bottom of the present invention is glass；ITO is completely covered by substrate as an electrode, electrocondution slurry in drop, and the electrode is drawn with wire.ITO residues are not covered as the part of electrode by layer of ZnO inculating crystal layer；Inculating crystal layer thickness is about 200 nm.It is the ZnO nano-rod array of epitaxial growth on ZnO inculating crystal layers, ZnO nano-rod array surface is coated by organic matter phenanthrene.The advantages of this ZnO nanorod of the present invention and the ultraviolet photovoltaic detector of luxuriant and rich with fragrance nano heterogeneous composite construction, low cost, easy realization, high efficiency, good stability, there is great application potential in the field such as military, civilian.
Description
Technical field
The invention belongs to semiconductor and nano photoelectronic devices field, more particularly to a kind of ZnO nanorod and luxuriant and rich with fragrance nanometer
The preparation method of the ultraviolet photovoltaic detector of Heterogeneous Composite structure.
Background technology
Photodetector is a kind of device that optical radiation signal is converted to electric signal, can be perceived using this characteristic outer
The change of boundary's environment.Ultraviolet light is that people can not with the naked eye observe directly, and radianting capacity is strong.In order to avoid people are by purple
The direct radiation of outer light, it is necessary to by the physical quantity changed this ultraviolet light for ease of detection.Ultraviolet photovoltaic detector is just
It is that a kind of sightless ultraviolet incident radiation signal can be converted to the device of detectable electric signal.Ultraviolet photovoltaic detector exists
Ultraviolet alarm and guidance are widely used in military affairs, while civilian aspect also relates to the fields such as ultraviolet monitoring and early warning.Cause
This, many countries have carried out deeply extensive research to ultraviolet photovoltaic detector, improve constantly the performance of ultraviolet photovoltaic detector
And stability, so as to provide safety guarantee for the country and people.
ZnO be it is a kind of there is photoelectricity, piezoelectricity, the semi-conducting material of catalysis, energy gap is 3.37 eV under normal temperature,
It is typical direct band gap semiconductor material with wide forbidden band, while exciton binding energy is up to 60 meV, with excellent luminescent properties,
It is adapted to the research of ultraviolet light photo devices field.
ZnO nanorod has the advantages that ZnO material itself, and the high intensity and high tenacity of nano material are combined again, is showed
Go out good ultraviolet detector performance and stability.But, be present a large amount of room trap states in ZnO nanorod surface, receive ultraviolet
The electron hole pair diffusion produced when light is excited is influenceed by surface depletion layer, and Carrier recombination is serious, causes ZnO nano
The detection performance of rod base ultraviolet light volt detector and sensitivity are low.
The content of the invention
Present invention aims at provide a kind of ultraviolet photovoltaic detector with ZnO nanorod and luxuriant and rich with fragrance Heterogeneous Composite structure and
Preparation method, detection performance and the sensitivity of current ZnO nanorod base ultraviolet light volt detector can be solved to a certain extent
Problem.
A kind of ultraviolet photovoltaic detector with ZnO nanorod with luxuriant and rich with fragrance nano heterogeneous composite construction, by substrate, positive and negative electrode
Layer, ultraviolet light functional layer are constituted, it is characterised in that substrate is sheet glass substrate；High work content material ITO is deposited on sheet glass substrate
It is used as negative electrode layer；The upper spin coating ZnO inculating crystal layers of negative electrode layer, are existed by hydro-thermal method epitaxial growth of ZnO nanometer stick array
On ZnO inculating crystal layers；With sol evenning machine spin coating luxuriant and rich with fragrance ethanol solution containing organic matter on ZnO nanometer stick arrays, drying substrate makes ethanol
Volatilization forms ZnO nanometer rods and luxuriant and rich with fragrance functional layer；Have respectively from drop in ITO the and ZnO nanometer rods and luxuriant and rich with fragrance functional layer of electrocondution slurry
Wire extraction electrode is used, ultraviolet photovoltaic detector structure of the present invention is formed.
Described electrocondution slurry is silver paste or conductive carbon pastes.
Described wire is spun gold or copper wire.
A kind of ultraviolet photovoltaic detector with ZnO nanorod with luxuriant and rich with fragrance nano heterogeneous composite construction of the present invention, its feature
It is what the detector was prepared by following method, comprises the following steps that：
The first step, cleans ito glass piece substrate：The sheet glass substrate that deposition has high work content material ITO is cleaned and dried；
Second step, prepares ZnO seed precursor solutions；Every gram of acetic acid dihydrate zinc adds ethanol 15-45 ml, monoethanolamine
0.25-0.75 ml, ethylene glycol 0.5-1.5 ml, stirring are dissolved completely in the mixed solution up to solute, add 0.25-
0.75ml glacial acetic acids, after being sufficiently stirred for, sealing ageing at least 12 h；
The ZnO seed precursor solutions prepared are spin-coated on by the 3rd step, spin coating ZnO precursor solution using spin coater
On ITO surfaces, and evaporate substrate solvent；
4th step, ZnO inculating crystal layer crystallization：ZnO inculating crystal layer sol evenning machines spin coating ZnO seed solutions on ITO, are obtained
Even ZnO inculating crystal layers, are brought rapidly up to 400 DEG C, are incubated 1-3 h, are cooled to room temperature and obtain ZnO inculating crystal layers；
5th step, hydro-thermal method epitaxial growth of ZnO nanometer stick array；
6th step, removal of impurities：Substrate is taken out, rinsed well, kept dry；
7th step, the luxuriant and rich with fragrance functional layer as device of being adulterated using spin-coating method in ZnO nano-rod array；
8th step, drips electrocondution slurry respectively on ITO and functional layer respectively, then with one end of two wires introduces every respectively
Drip in electrocondution slurry, the other end is hanging, form the both positive and negative polarity of ultraviolet detector.
The device of extraction electrode is fixed on test board by described ultraviolet photovoltaic detector, then by ZnO nanorod with it is luxuriant and rich with fragrance
The place for being partially disposed in luminous energy irradiation of electrode in functional layer, with the performance test of convenient device.
The ultraviolet photovoltaic detector structure of the present invention, the base material of the bottom is glass；ITO covers completely as an electrode
It is placed in substrate, electrocondution slurry in drop draws the electrode with wire.ITO residues are not as the part of electrode by layer of ZnO seed crystal
Layer covering；Inculating crystal layer thickness is about 200 nm.It is the ZnO nano-rod array of epitaxial growth on ZnO inculating crystal layers.By ZnO inculating crystal layers
Substrate vertical immersion in acetic acid dihydrate zinc（Zn（CH3COO）2·2H2O）And hexamethylenetetramine（HTM）Mixed aqueous solution
Middle epitaxial growth（002）ZnO nano-rod array in orientation；The a diameter of 50-200 nm of ZnO nanorod, length is 2-3 μm.
ZnO nano-rod array surface is coated by organic matter phenanthrene.
The preferred orientation of ZnO nanorod of the present invention ensure that carrier along ZnO nanorod perpendicular to substrate direction
Transmission, is conducive to improving photoelectric efficiency.ZnO nanometer stick arrays ensure that ZnO nanorod is heterogeneous with phenanthrene with the compound of organic matter phenanthrene
The formation of knot, so as to provide condition for the generation of photo-generated carrier.
In the present invention, broad stopband ZnO semi-conducting materials are selected, the photodetector can be effectively filtered out to visible
The response of light.Organic matter selection is luxuriant and rich with fragrance, is similarly due to that phenanthrene only can be to ultraviolet light response.ZnO is combined with luxuriant and rich with fragrance, can either be ensured
The active layer filtering of device is infrared and visible ray is only to ultraviolet light response, both can be combined again ultraviolet light is effectively inhaled
Receive.Both the characteristic of ZnO material and the stability of nano material had been combined, but also with organic-inorganic heterogeneous efficient photism
Can, considerably improve detection performance and the sensitivity of ultraviolet photovoltaic detector.ZnO nanorod and luxuriant and rich with fragrance nano heterogeneous composite construction
Excellent performance is shown as the functional layer of ultraviolet photovoltaic detector, D* is up to 9.0 × 10 for its detectivity13Jones（1
Jones=1 cm Hz1/2 W-1）；R is up to 2.0 × 10 for sensitivity response rate4 A/W。
This ZnO nanorod of the present invention and the ultraviolet photovoltaic detector of luxuriant and rich with fragrance nano heterogeneous composite construction, low cost, Yi Shi
Now, the advantages of high efficiency, stability are good, has great application potential in the field such as military, civilian.
Brief description of the drawings
Fig. 1 is ultraviolet photovoltaic detector structural representation of the present invention；
Fig. 2 a are the plane SEM figures of the ultraviolet photovoltaic detector ZnO nano-rod array of embodiment 2；
Fig. 2 b are the section SEM figures of the ultraviolet photovoltaic detector ZnO nano-rod array of embodiment 2；
Fig. 3 a are the plane SEM figures of the ultraviolet photovoltaic detector ZnO nano-rod array of embodiment 3/phenanthrene functional layer；
Fig. 3 b are the section SEM figures of the ultraviolet photovoltaic detector ZnO nano-rod array of embodiment 3/phenanthrene functional layer；
Fig. 4 is ultraviolet-visible-infrared absorpting light spectra of Fig. 2 and 3 ultraviolet light absorption materials；
Fig. 5 is the J-V curves of the ultraviolet photovoltaic detector of embodiment 1；
Fig. 6 is the responsiveness curve of the ultraviolet photovoltaic detector of embodiment 1；
Fig. 7 is the detectivity curve of the ultraviolet photovoltaic detector of embodiment 1.
Wherein, in Fig. 1：Ultraviolet source 1, substrate 2, negative electrode 3, ZnO of layer inculating crystal layers 4, ZnO nanometer stick arrays 5, ZnO
Nanometer rods and luxuriant and rich with fragrance functional layer 6, electrocondution slurry 7, wire 8.
Embodiment
In order that the purpose of the present invention, preparation method and advantage are clearer, in conjunction with the following drawings and embodiment, to this
Invention more illustrate in detail.
Embodiment 1：A kind of ultraviolet photovoltaic detector with ZnO nanorod and luxuriant and rich with fragrance nano heterogeneous composite construction, substrate 2 is
Sheet glass substrate；The thick high work content material ITO of 180 nm are deposited on sheet glass substrate as negative electrode layer 3；Negative electrode layer 3
The upper nm of spin coating 200 ZnO inculating crystal layers 4, are 2-3 μm of ZnO by a diameter of 50-200 nm of hydro-thermal method epitaxial growth, length
Nanometer stick array 5 is on ZnO inculating crystal layers 4；With sol evenning machine spin coating luxuriant and rich with fragrance ethanol solution containing organic matter in ZnO nanometer stick arrays 5
On, drying substrate makes ethanol volatilize to form ZnO nanometer rods and luxuriant and rich with fragrance functional layer 6；There is the ITO negative electrodes layer of silver paste 7 from drop respectively
3rd, ZnO nanometer rods form ultraviolet photovoltaic detector structure of the present invention with using the extraction electrode of spun gold wire 8 in luxuriant and rich with fragrance functional layer 6.
The ultraviolet photovoltaic detector of the present invention, is prepared by following technique, comprised the following steps that：
The first step, cleans ito glass piece substrate：The thick high work content material ITO of 180 nm sheet glass substrate will be deposited with washing
Wash agent, acetone（AR）, ethanol（AR）It is cleaned by ultrasonic 10 min respectively in order, then with deionized water rinse substrate, drying repeatedly
Preserve substrate.
Second step, prepares ZnO seed precursor solutions：By the g of acetic acid dihydrate zinc 2, the ml of monoethanolamine 1, the ml of ethylene glycol 2,
It is dissolved into successively in the ml of ethanol 60, adds the ml of glacial acetic acid 1, after being sufficiently stirred for, 12 h of sealing ageing.
3rd step, spin coating ZnO precursor solution：Ito glass piece substrate is transferred on sol evenning machine up, pipette is used
The ZnO seed precursor solutions for drawing 100 μ L are dropped on ITO surfaces, after solution is paved with ITO surfaces completely, is prewhirled and are coated with
1000 rpm speed rotate 3 s, and spin coating rotates 30 s with 4000 rpm speed, and hair-dryer hot blast is used after the completion of spin coating against substrate
Blow 3-5 min in the back side so that solvent evaporates.
4th step, ZnO inculating crystal layer crystallization：The substrate that above-mentioned 3rd step is obtained is transferred in quartz ampoule, then quartz ampoule is put
In quick anneal oven, stove rises to 400 DEG C with 20 DEG C/min speed, is incubated 2 h, quartz ampoule is taken out afterwards, at room temperature certainly
So 30 min of cooling, obtain the ZnO inculating crystal layers of the thick crystallization of 200 nm.
5th step, Hydrothermal Growth ZnO nano-rod array：ZnO nanorod reaction solution is poured into closed container, is preheating to
50 DEG C, the substrates of ZnO inculating crystal layers is then will be covered with again and is placed perpendicular to container bottom, then be warming up to 90 DEG C, be incubated 6 h, stop
Only heat, reaction system be placed in the h of natural cooling 2 under room temperature condition, obtain a diameter of 50-200 nm that Hydrothermal Growth goes out,
Length is 2-3 μm of ZnO nano-rod array.Wherein, the preparation of reaction solution：0.004 mol acetic acid dihydrate zinc（Zn
（CH3COO）2·2H2O）With 0.004 mol hexamethylenetetramines（HTM）It is dissolved in 0.2 L deionized waters, in hydro-thermal reaction system
Reaction solution concentration be 0.02 mol/L.
6th step, removal of impurities：The substrate taking-up for having ZnO nano-rod array will be grown, rinsed repeatedly with deionized water 5 times, then
Substrate is dried up with hair-dryer, kept dry.
7th step, doping is luxuriant and rich with fragrance：The luxuriant and rich with fragrance ethanol solutions of 0.2 mol/L are prepared, take the 50 μ L solution to drip in growth with pipettor
Have on ZnO nano-rod array, after being paved with, 30s is rotated with 1000 rpm speed.Substrate is transferred in heating plate again, made
Ethanol volatilizees, and obtains the luxuriant and rich with fragrance ZnO nano-rod array of doping as active layer, the dry Cord blood substrate.
8th step, draws electrode：Silver paste is dripped on ITO, ZnO nanorod battle array/luxuriant and rich with fragrance active layer respectively, then respectively with two
One end of spun gold wire is introduced into often drop silver paste, and the other end is hanging, forms the positive and negative electrode of ultraviolet detector.
9th step, assembly device：The device of extraction electrode is fixed on test board, makes silver electrode on luxuriant and rich with fragrance active layer
The place that ultraviolet source 1 can irradiate is partially disposed in, with the test performance of convenient device.
Embodiment 2：（1）With sol evenning machine on ITO spin coating ZnO seed solutions, obtain uniform ZnO inculating crystal layers, Ran Hou
Annealing obtains the nm of thickness about 200 ZnO inculating crystal layers under air atmosphere；（2）On ZnO inculating crystal layers, hydro-thermal method epitaxial growth is utilized
Go out the ZnO nano-rod array of orientation, form uniform ZnO nano-rod array.Nanorod diameter is 50-200nm, and length is 2-3 μ
m.Other step be the same as Examples 1.
Embodiment 3：Sol evenning machine is borrowed by luxuriant and rich with fragrance ethanol solution with spin coating mode spin coating, 50 μ L luxuriant and rich with fragrance ethanol solution is dripped
Substrate is paved with, the rotating speed of regulation sol evenning machine rotates 30s for 1000 rpm so that luxuriant and rich with fragrance ethanol solution is fully seeped into ZnO nanorod
In array, 30 min in 80 DEG C of heating plate are then placed the substrate in so that ethanol solution can be sent out completely, and phenanthrene is coated on ZnO and received
Rice rod surface, obtains ZnO nanorod and luxuriant and rich with fragrance nano heterogeneous composite construction.
Claims (6)
1. a kind of ultraviolet photovoltaic detector with ZnO nanorod with luxuriant and rich with fragrance nano heterogeneous composite construction, by substrate, positive and negative electrode
Layer, ultraviolet light functional layer are constituted, substrate（2）For sheet glass substrate；High work content material ITO is deposited on sheet glass substrate and is used as negative pole
Electrode layer（3）；Negative electrode layer（3）Upper spin coating ZnO inculating crystal layers（4）, pass through hydro-thermal method epitaxial growth of ZnO nanometer stick array（5）
In ZnO inculating crystal layers（4）On；With sol evenning machine spin coating luxuriant and rich with fragrance ethanol solution containing organic matter in ZnO nanometer stick arrays（5）On, dry base
Piece makes ethanol volatilize to form ZnO nanometer rods and luxuriant and rich with fragrance functional layer（6）；There is electrocondution slurry from drop respectively（7）ITO and ZnO nanometers
Rod and luxuriant and rich with fragrance functional layer（6）On use wire（8）Extraction electrode, forms ultraviolet photovoltaic detector structure of the present invention；Wherein, electrocondution slurry
（7）For silver paste or conductive carbon pastes, wire（8）For spun gold or copper wire；It is characterized in that the detector passes through following method system
Obtained by standby, comprise the following steps that：
The first step, cleans ito glass piece substrate：The sheet glass substrate that deposition has high work content material ITO is cleaned and dried；
Second step, prepares ZnO seed precursor solutions；Every gram of acetic acid dihydrate zinc adds ethanol 15-45 ml, monoethanolamine 0.25-
0.75 ml, ethylene glycol 0.5-1.5 ml, stirring are dissolved completely in the mixed solution up to solute, add 0.25-0.75ml ice
Acetic acid, after being sufficiently stirred for, sealing ageing at least 12 h；
The ZnO seeds precursor solution prepared is spin-coated on ITO tables by the 3rd step, spin coating ZnO precursor solution using spin coater
On face, and evaporate substrate solvent；
4th step, ZnO inculating crystal layer crystallization：ZnO inculating crystal layer sol evenning machines spin coating ZnO seed solutions on ITO, obtain uniform
ZnO inculating crystal layers, are brought rapidly up to 400 DEG C, are incubated 1-3 h, are cooled to room temperature and obtain ZnO inculating crystal layers；
5th step, hydro-thermal method epitaxial growth of ZnO nanometer stick array；
6th step, removal of impurities：Substrate is taken out, rinsed well, kept dry；
7th step, the luxuriant and rich with fragrance functional layer as device of being adulterated using spin-coating method in ZnO nano-rod array；
8th step, drips electrocondution slurry, then introduces often drop with one end of two wires respectively and lead respectively on ITO and functional layer respectively
In plasma-based material, the other end is hanging, forms the both positive and negative polarity of ultraviolet detector.
2. a kind of ultraviolet photovoltaic detector with ZnO nanorod with luxuriant and rich with fragrance nano heterogeneous composite construction as claimed in claim 1,
It is characterized in that it is addition monoethanolamine 0.5 ml, ethylene glycol in every gram of acetic acid dihydrate zinc to prepare ZnO seed precursor solutions
1ml, is dissolved into the ml of ethanol 30, adds glacial acetic acid 0.5ml successively, after being sufficiently stirred for, 12 h of sealing ageing.
3. a kind of ultraviolet photovoltaic detector with ZnO nanorod with luxuriant and rich with fragrance nano heterogeneous composite construction as claimed in claim 1,
It is characterized in that spin coating ZnO precursor solution is to be transferred to ito glass piece substrate on sol evenning machine up, pipette, extract is used
100 μ L ZnO seed precursor solutions are dropped on ITO surfaces, after solution is paved with ITO surfaces completely, is prewhirled and are coated with 1000
Rpm speed rotates 3s, and spin coating rotates 30 s with 4000 rpm speed, blown after the completion of spin coating with hair-dryer hot blast against backside of substrate
3-5 min so that solvent evaporates.
4. a kind of ultraviolet photovoltaic detector with ZnO nanorod with luxuriant and rich with fragrance nano heterogeneous composite construction as claimed in claim 1,
It is characterized in that ZnO inculating crystal layer crystallization is that substrate is transferred in quartz ampoule, then quartz ampoule is placed in quick anneal oven, stove
400 DEG C are risen to 20 DEG C/min speed, 2 h is incubated, quartz ampoule is taken out afterwards, the min of natural cooling 30, obtains 200 at room temperature
The ZnO inculating crystal layers of nm thickness crystallization.
5. a kind of ultraviolet photovoltaic detector with ZnO nanorod with luxuriant and rich with fragrance nano heterogeneous composite construction as claimed in claim 1,
It is characterized in that Hydrothermal Growth ZnO nano-rod array is to pour into ZnO nanorod reaction solution in closed container, 50 are preheating to
DEG C, the substrates of ZnO inculating crystal layers then will be covered with again and is placed perpendicular to container bottom, then be warming up to 90 DEG C, be incubated 6h, stop plus
Heat, the h of natural cooling 2 under room temperature condition is placed in by reaction system, obtains a diameter of 50-200 nm, length that Hydrothermal Growth goes out
For 2-3 μm of ZnO nano-rod array；
Wherein, the preparation of reaction solution：0.004 mol acetic acid dihydrate zinc（Zn（CH3COO）2·2H2O）With 0.004 mol six times
Tetramine（HTM）It is dissolved in 0.2 L deionized waters, the reaction solution concentration in hydro-thermal reaction system is 0.02 mol/L.
6. a kind of ultraviolet photovoltaic detector with ZnO nanorod with luxuriant and rich with fragrance nano heterogeneous composite construction as claimed in claim 1,
It is characterized in that doping phenanthrene is to take the 50 μ L solution to drip with pipettor the ethanol solution of 0.2 mol/L phenanthrene to have ZnO to receive in growth
On rice rod array, after being paved with, 30s is rotated with 1000 rpm speed.
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| CN107287615B (en) * | 2017-06-01 | 2019-10-11 | 北京科技大学 | A kind of vanadium doping ZnO nano-rod array light anode and its preparation method and application |
| CN109103212B (en) * | 2018-08-03 | 2020-07-10 | 中国科学院金属研究所 | Flexible image sensor based on hair and manufacturing method thereof |
| CN112599622B (en) * | 2020-12-15 | 2023-09-26 | 广西大学 | Sandwich structure array type porous ultraviolet photoelectric detector and preparation method thereof |
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| CN101214989A (en) * | 2007-12-28 | 2008-07-09 | 中山大学 | Process for preparing nano structure of zinc oxide |
| CN101976728A (en) * | 2010-09-29 | 2011-02-16 | 昆明物理研究所 | Photovoltaic organic ultraviolet semiconductor detector |
| CN102222771A (en) * | 2011-06-30 | 2011-10-19 | 昆明物理研究所 | Organic and inorganic hybridized semiconductor ultraviolet photovoltaic detector |
| CN102492987A (en) * | 2011-12-23 | 2012-06-13 | 南京工业大学 | Process for growth of ZnO nano-wire array on flexible substrate by using solution method |
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| KR20130029247A (en) * | 2011-09-14 | 2013-03-22 | 삼성전자주식회사 | Organic solar cell and method of manufacturing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101214989A (en) * | 2007-12-28 | 2008-07-09 | 中山大学 | Process for preparing nano structure of zinc oxide |
| CN101976728A (en) * | 2010-09-29 | 2011-02-16 | 昆明物理研究所 | Photovoltaic organic ultraviolet semiconductor detector |
| CN102222771A (en) * | 2011-06-30 | 2011-10-19 | 昆明物理研究所 | Organic and inorganic hybridized semiconductor ultraviolet photovoltaic detector |
| CN102492987A (en) * | 2011-12-23 | 2012-06-13 | 南京工业大学 | Process for growth of ZnO nano-wire array on flexible substrate by using solution method |
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