CN105244440B - A kind of flexible thin film type PEDOT ZnO ultraviolet light detectors and preparation method thereof - Google Patents
A kind of flexible thin film type PEDOT ZnO ultraviolet light detectors and preparation method thereof Download PDFInfo
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- CN105244440B CN105244440B CN201510603894.8A CN201510603894A CN105244440B CN 105244440 B CN105244440 B CN 105244440B CN 201510603894 A CN201510603894 A CN 201510603894A CN 105244440 B CN105244440 B CN 105244440B
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
- H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
- H10K85/113—Heteroaromatic compounds comprising sulfur or selene, e.g. polythiophene
- H10K85/1135—Polyethylene dioxythiophene [PEDOT]; Derivatives thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The present invention relates to a kind of flexible thin film type PEDOT ZnO ultraviolet light detectors and preparation method thereof, the ultraviolet light detector is photoconduction type ultraviolet light detector, including flexible photosensitive film and the electrode on film；Specifically, described flexible photosensitive film is the PEDOT ZnO films being spin-coated on transparent flexible plastic film, count in mass ratio, PEDOT and ZnO ratio are 7:1.Described electrode is Au/Ti interdigital electrodes；There is potential barrier between pure PEDOT and ZnO material, photoconductive property to both composite systems has a strong impact on, material in preparation method of the present invention have passed through the doping based on band engineering design, both original interface potential barriers are eliminated, make PEDOT ZnO flexible thin film type ultraviolet light detectors that there is outstanding photoconductive response characteristic.
Description
Technical field
The present invention relates to semi-conducting material and its preparation field, and in particular to a kind of flexible thin film type PEDOT-ZnO is ultraviolet
Photo-detector and preparation method thereof.
Background technology
Ultraviolet light detector has very high application value in many application scenarios.Military aspect can be used for aerospace detection,
Fighter plane tail flame tracking, Missile Plume tracking etc.；Civilian aspect can be used for high-voltage corona detection, ultraviolet fingerprint detection, flame to visit
Survey etc..Semiconductor ultraviolet detector performance is stable, easy to use, in having been widely used for producing and living.But, at present
The ultraviolet light detector prepared with semi-conducting material is mostly rigid solid, it is impossible to which bending is folded, and needs to carry out phase at some
Inconvenience is installed and used to the equipment privileged sites of motion.Develop can arbitrarily folded bent flexible thin film type ultraviolet light detector,
It can overcome the disadvantages that the deficiency of the rigid ultraviolet light detector of conventional semiconductor in this regard.
PEDOT (poly- 3,4- ethylenedioxy thiophenes) is a kind of macromolecule organic semiconducting materials.With conductance height, environment
Stability is good, it is cheap the advantages of.PEDOT has good pliability, can arbitrarily be bent in the case where thickness is little
Fold.
The content of the invention
For defect of the prior art and deficiency, there is outstanding responsiveness ability it is an object of the invention to provide one kind
Flexible thin film type ultraviolet light detector and preparation method thereof.
The concrete technical scheme of the present invention：
A kind of flexible thin film type PEDOT-ZnO ultraviolet light detectors, including flexible substrates, photo-conductive film and electrode；It is described
Photo-conductive film include PEDOT：PSS and zinc oxide mixture, and the doping Na and N in zinc oxide.
Specifically, counting in mass ratio, PEDOT and ZnO ratio is 7 in photo-conductive film:1；By atomic mass percentages,
The amount that doping Na amount is doping N in 5%, zinc oxide in zinc oxide is 6%；By mass percentage, PEDOT：PSS in PSS
Incorporation be 1.6%.
More specifically, described flexible substrates are polyethylene terephthalate film, and described electrode is interdigital for Au/Ti
Electrode.
The method for preparing described flexible thin film type PEDOT-ZnO ultraviolet light detectors, including use collosol and gel legal system
Standby doping Na and N ZnO, by doped with Na and N ZnO and PEDOT:PSS is prepared into colloid mixture, and colloid mixture is spin-coated on
Electrode is prepared on a flexible substrate in flexible substrates and by cosputtering method, produces PEDOT-ZnO flexible thin film type ultraviolet lights
Detector.
Specifically, the ZnO that described sol-gal process prepares doping Na and N is included with acetic acid zinc solution, sodium nitrate solution
Be prepared by raw material with ammonium acetate solution, acetic acid zinc concentration is 0.01mol/L, the concentration of sodium nitrate for 0.001~
0.01mol/L, the concentration of ammonium acetate is 0.01~0.1mol/L.
Further, by doped with Na and N ZnO material and PEDOT:PSS be prepared into before colloid mixture to doped with
Na and N ZnO is heat-treated, and it is 1 that described heat treatment condition, which includes oxygen and argon pressure ratio,:1 atmosphere and 800 DEG C.
More specifically, by doped with the ZnO powder and PEDOT that Na and N particle diameter are 200~800nm:It is prepared by PSS
Into colloid mixture.
Again specifically, described cosputtering prepares the method for electrode using Au targets and Ti palladiums under 20Pa argon atmospheres
Cosputtering makes Au/Ti electrodes on a flexible substrate.
Beneficial effects of the present invention are：
(1) there is potential barrier, the photoconductive property to both composite systems has between pure PEDOT and ZnO material
And have a strong impact on, the material in preparation method of the present invention have passed through the doping based on band engineering design, eliminate both original
Interface potential barrier, make PEDOT-ZnO flexible thin film type ultraviolet light detectors that there is outstanding photoconductive response characteristic；
(2) with compared with size, the device based on single PEDOT or ZnO material of similar shape, prepared by the present invention
PEDOT-ZnO composite devices have more excellent light sensitive characteristic.The device of single PEDOT systems is almost without ultraviolet sound
Should, the devices of ZnO systems has a ultraviolet response, and compared with the above two PEDOT-ZnO composites device ultraviolet light response
Degree improves highly significant；
(3) PEDOT-ZnO flexible thin film type ultraviolet light detectors prepared by the present invention are a kind of flexible semiconductor ultraviolet lights
Detector, it is mostly rigid device to solve existing semiconductor ultraviolet detector, needs to carry out relative motion at some
The problem of equipment privileged sites install and use inconvenience, while the photo-conductive film of conventional rigid semiconductor photo-detector is required for greatly
Prepared by vacuum system, equipment costliness causes preparation cost very high, and the photo-conductive film preparation process of this preparation method core is without true
Altitude, flow is simple, with low cost.
Brief description of the drawings
Fig. 1 is the brightness IV curves of PEDOT-ZnO flexible thin film type ultraviolet light detectors prepared by embodiment one；
Fig. 2 is the response spectra of PEDOT-ZnO flexible thin film type ultraviolet light detectors prepared by embodiment one；
The present invention is illustrated below in conjunction with specification drawings and specific embodiments.
Embodiment
Existing semiconductor ultraviolet detector is mostly rigid device, needs the equipment for carrying out relative motion special at some
Inconvenience is installed and used at different position, and based on this, the present invention is prepared using PEDOT (poly- 3,4-ethylene dioxythiophene) together with zinc oxide
Into soft ultraviolet light detector, the ultraviolet light detector is photoconduction type ultraviolet light detector, photoconduction type ultraviolet detector
Device includes flexible substrates, photo-conductive film and electrode；Photo-conductive film spin coating on a flexible substrate, by electrode be connected with photo-conductive film into
Row is conductive, but finds there is potential barrier between pure PEDOT and ZnO material during the preparation, to both composites
The photoconductive property of system has a strong impact on；
What use organic semiconducting materials PEDOT and inorganic semiconductor material ZnO proposed by the present invention were combined into
PEDOT-ZnO flexible thin film type ultraviolet light detectors and preparation method thereof, have not yet to see same or like patent and document
Report；The technical problem to be solved in the present invention is that solving PEDOT/ZnO interfacial states and interface potential barrier using doping influences device light
The problem of quick performance because interfacial state and interface potential barrier when can cause the electronics to be transported between ZnO and PEDOT by serious
Block, and many photo-generated carriers are consumed by Interface composites, so as to seriously reduce photoelectric current and cause current-voltage correlation non-
Linearisation, influences the photosensitive property of photoconductive detector.PEDOT-ZnO fexible films are prepared using spin-coating method, and are prepared
PEDOT-ZnO flexible thin film type ultraviolet light detectors with outstanding photosensitive property.
In face of above-mentioned difficulties, invention human desires overcomes above mentioned problem by adulterating other elements in zinc oxide material, leads to
Substantial amounts of experiment screening is crossed to find, by Na and N co-dopeds enter after zinc oxide material with after doping PSS (polystyrolsulfon acid)
PEDOT is PEDOT:PSS materials are prepared into the ultraviolet light detector of flexibility together, solve pure PEDOT and ZnO material it
Between have Potential Barrier Problems；
PEDOT:PSS is the PEDOT high molecular polymers after doping PSS, with excellent conductance.With doping PSS
Amount it is different materials conductive rate it is also different.The PEDOT that the present invention is used:PSS solution is limited purchased from Wuhan Si Nuofuhong science and technology
Company.
The ultraviolet light detector of the present invention is photoconduction type ultraviolet light detector, and photoconduction type ultraviolet light detector includes soft
Property photo-conductive film and the electrode on film, flexible photosensitive film is that the PEDOT-ZnO being spin-coated on transparent flexible plastic film is thin
Film, is counted in mass ratio, and PEDOT and ZnO ratio are 7:1；Na and atomic mass percentages of the N in zinc oxide are respectively 5%
With 6%, electrode is Au/Ti interdigital electrodes；By mass percentage, PEDOT：PSS incorporation is 1.6% in PSS materials.
The preparing raw material and preparation method of the ultraviolet light detector of the present invention are done specifically below in conjunction with specific embodiment
It is bright：
Embodiment 1：
Step 1：Sol-gal process is used to prepare the ZnO material of doping by raw material of zinc acetate, sodium nitrate and ammonium acetate,
Step is as follows：Configuration contains 0.01mol/L zinc acetates, 0.001mol/L sodium nitrate and 0.01mol/L ammonium acetate mixed solutions, plus
Heat to addition PVA to concentration 0.5g/L after 90 degrees Celsius, stirring stands to stirring at normal temperature and forms ZnO colloid in 1 hour for 2 hours again.
Colloid is placed in glass, oven for drying is put into.
Step 2：ZnO after drying is put into atmosphere furnace, is 1 in pressure ratio:Carried out in 1 oxygen and argon atmosphere
800 DEG C of heat treatments.ZnO is put into ball mill again, the ball mill of the cycle per minute clock of frequency 1200 is shaken by after heat treatment using pendulum
ZnO is milling 72 hours, obtains average particulate diameter about 500nm ZnO:(Na, N) powder.
Step 3：By ZnO:(Na, N) powder and PEDOT:(Wuhan Si Nuofuhong Science and Technology Ltd.s produce PSS, PEDOT:
PSS water solubilitys stoste) mixing, count in mass ratio, PEDOT and ZnO ratio are 7:1.Colloid is spin-coated on transparent flexible plastic
On film, PEDOT-ZnO flexible photosensitive films are obtained.
Step 4：Saturating PEDOT-ZnO flexible photosensitives film is put into sputtering system, using Au targets and Ti palladiums in argon atmosphere
Lower cosputtering, air pressure 20Pa makes Au/Ti interdigital electrodes.So as to complete PEDOT-ZnO flexible thin film type ultraviolet light detectors
Prepare.
Fig. 1 is the brightness IV curves of PEDOT-ZnO flexible thin film type ultraviolet light detectors prepared by the inventive method, and it shines
Light source is penetrated for ultraviolet mercury lamp.It can be seen from the figure that sample under ultraviolet irradiation generates obviously photoelectric current, and IV
Curve is straight line, complies fully with the feature of photoconduction type ultraviolet detector.Fig. 2 is that PEDOT-ZnO prepared by the inventive method is soft
Property film-type ultraviolet light detector response spectra, it can be seen that it has very strong sound to wavelength less than 360nm ultraviolet radiation
Should, but the visible ray that wavelength is more than 400nm is not almost responded to, illustrate that it has outstanding optical electivity targetedly ultraviolet
Detecting function.Table 1 gives responsiveness of the PEDOT-ZnO flexible thin film type ultraviolet light detectors of the present embodiment at 360nm
Concrete numerical value.
Embodiment 2：
Preparation method and test be the same as Example 1, but solution concentration change is prepared in step 1 and turns to 0.01mol/L acetic acid
Zinc, 0.01mol/L sodium nitrate, 0.01mol/L ammonium acetate mixed solutions.Table 1 gives this ultraviolet detector prepared by real-time example
The numerical value of device responsiveness, the response performance of the ultraviolet light detector of the present embodiment is poor compared with embodiment 1 as can be seen from Table 1.
Embodiment 3：
Preparation method and test be the same as Example 1, but solution concentration change is prepared in step 1 and turns to 0.01mol/L acetic acid
Zinc, 0.001mol/L sodium nitrate, 0.1mol/L ammonium acetate mixed solutions.Table 1 gives this ultraviolet detector prepared by real-time example
The numerical value of device responsiveness, the response performance of the ultraviolet light detector of the present embodiment is poor compared with embodiment 1 as can be seen from Table 1.
Embodiment 4：
Preparation method and test be the same as Example 1, but eliminate the heat treatment link in step 2.Table 1 gives this in real time
The response of the numerical value, the as can be seen from Table 1 ultraviolet light detector of the present embodiment of ultraviolet light detector responsiveness prepared by example
Can be poor compared with embodiment 1.
Embodiment 5：
Preparation method and test be the same as Example 1, but eliminate the ball mill in step 2 and mill link.Table 1 gives this
The sound of the numerical value, the as can be seen from Table 1 ultraviolet light detector of the present embodiment of ultraviolet light detector responsiveness prepared by real-time example
Answer performance poor compared with embodiment 1.
Embodiment 6：
Preparation method and test be the same as Example 1, but PEDOT and ZnO ratio is 14 in step 3:1.Table 1 gives this
The sound of the numerical value, the as can be seen from Table 1 ultraviolet light detector of the present embodiment of ultraviolet light detector responsiveness prepared by real-time example
Answer performance poor compared with embodiment 1.
Embodiment 7：
Preparation method and test be the same as Example 1, but PEDOT and ZnO ratio is 3 in step 3:1.Table 1 gives this
The sound of the numerical value, the as can be seen from Table 1 ultraviolet light detector of the present embodiment of ultraviolet light detector responsiveness prepared by real-time example
Answer performance poor compared with embodiment 1.
Embodiment 8：
Preparation method and test be the same as Example 1, but eliminate the link for PEDOT and ZnO being mixed in step 3, but
Only prepare rigid ZnO ultraviolet light detectors on the glass sheet with ZnO spin coatings.Table 1 gives the ultraviolet of this real-time example preparation
The numerical value of photo-detector responsiveness, the response performance of the ultraviolet light detector of the present embodiment is compared with embodiment 1 as can be seen from Table 1
Difference.
Embodiment 9：
Preparation method and test be the same as Example 1, but eliminate the link for PEDOT and ZnO being mixed in step 3, but
Only prepare rigid ZnO ultraviolet light detectors on the glass sheet with PEDOT spin coatings.Table 1 gives this purple prepared by real-time example
The numerical value of outer photo-detector responsiveness, as can be seen from Table 1 the present embodiment almost do not respond to.
Embodiment 10：
Preparation method and test be the same as Example 1, but step 1 does not add sodium nitrate and ammonium acetate, that is to say prepared
ZnO is undoped.Table 1 gives the numerical value of this ultraviolet light detector responsiveness prepared by real-time example, as can be seen from Table 1 this reality
The response performance for applying the ultraviolet light detector of example is poor compared with embodiment 1.
Embodiment 11：
Preparation method and test be the same as Example 1, but step 1 does not add sodium nitrate, that is to say prepared ZnO without mixing
Miscellaneous Na.Table 1 gives the numerical value of ultraviolet light detector responsiveness prepared by this real-time example, as can be seen from Table 1 the present embodiment
The response performance of ultraviolet light detector is poor compared with embodiment 1.
Embodiment 12：
Preparation method and test be the same as Example 1, but step 1 does not add ammonium acetate, that is to say prepared ZnO without mixing
Miscellaneous N.Table 1 gives the purple of the numerical value, as can be seen from Table 1 the present embodiment of this ultraviolet light detector responsiveness prepared by real-time example
The response performance of outer photo-detector is poor compared with embodiment 1.
Table 1
| Embodiment | Responsiveness (A/W) |
| 1 | 2.23 |
| 2 | 1.63 |
| 3 | 1.26 |
| 4 | 1.58 |
| 5 | 1.79 |
| 6 | 1.24 |
| 7 | 1.17 |
| 8 | 0.95 |
| 9 | 0.02 |
| 10 | 0.68 |
| 11 | 0.75 |
| 12 | 0.82 |
Claims (7)
1. a kind of flexible thin film type PEDOT-ZnO ultraviolet light detectors, it is characterised in that including flexible substrates, photo-conductive film and
Electrode；
Described photo-conductive film includes PEDOT：PSS and zinc oxide mixture, and the doping Na and N in zinc oxide；
Count in mass ratio, PEDOT and ZnO ratio is 7 in photo-conductive film:1；By atomic mass percentages, mixed in zinc oxide
The amount that miscellaneous Na amount is doping N in 5%, zinc oxide is 6%；By mass percentage, PEDOT：PSS incorporation is in PSS
1.6%.
2. flexible thin film type PEDOT-ZnO ultraviolet light detectors as claimed in claim 1, it is characterised in that described flexibility
Substrate is polyethylene terephthalate film, and described electrode is Au/Ti interdigital electrodes.
3. prepare the method for the flexible thin film type PEDOT-ZnO ultraviolet light detectors described in claim 1 or 2, it is characterised in that
ZnO including preparing doping Na and N using sol-gal process, by doped with Na and N ZnO and PEDOT:PSS is prepared into mixing
Colloid, prepares on a flexible substrate and on a flexible substrate electrode by cosputtering method by colloid mixture spin coating, produces
PEDOT-ZnO flexible thin film type ultraviolet light detectors.
4. the method as claimed in claim 3 for preparing flexible thin film type PEDOT-ZnO ultraviolet light detectors, it is characterised in that
The ZnO that described sol-gal process prepares doping Na and N is included using acetic acid zinc solution, sodium nitrate solution and ammonium acetate solution as original
Prepared by material, acetic acid zinc concentration is 0.01mol/L, and the concentration of sodium nitrate is 0.001~0.01mol/L, ammonium acetate it is dense
Spend for 0.01~0.1mol/L.
5. the method as claimed in claim 3 for preparing flexible thin film type PEDOT-ZnO ultraviolet light detectors, it is characterised in that
By doped with Na and N ZnO and PEDOT:PSS is prepared into before colloid mixture to be heat-treated to the ZnO doped with Na and N,
It is 1 that described heat treatment condition, which includes oxygen and argon pressure ratio,:1 atmosphere and 800 DEG C.
6. the method as claimed in claim 3 for preparing flexible thin film type PEDOT-ZnO ultraviolet light detectors, it is characterised in that
By doped with the ZnO powder and PEDOT that Na and N particle diameter are 200~800nm:PSS is prepared into colloid mixture.
7. the method as claimed in claim 3 for preparing flexible thin film type PEDOT-ZnO ultraviolet light detectors, it is characterised in that
Described cosputtering prepare the method for electrode using Au targets and Ti targets under 20Pa argon atmospheres cosputtering in flexible substrates
On make Au/Ti electrodes.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131254A (en) * | 2013-02-05 | 2013-06-05 | 陕西科技大学 | Zinc-oxide-containing dual-wavelength light-absorption aquosity anti-forgery ink easer preparation technology |
| CN103594631A (en) * | 2013-06-25 | 2014-02-19 | 北京科技大学 | Novel self-driven ultraviolet detector and manufacturing method thereof |
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|---|---|---|---|---|
| CN103131254A (en) * | 2013-02-05 | 2013-06-05 | 陕西科技大学 | Zinc-oxide-containing dual-wavelength light-absorption aquosity anti-forgery ink easer preparation technology |
| CN103594631A (en) * | 2013-06-25 | 2014-02-19 | 北京科技大学 | Novel self-driven ultraviolet detector and manufacturing method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 《Dual acceptor doping and aging effect of p-ZnO-(Na, N) nanorod thin films by spray pyrolysis》;R. Swapna, et al.;《AIP Conference Proceedings》;20150228;第1576卷(第1期);167-170 * |
| Tursun Abdiryim, et al..《A facile solid-state heating method for preparation of poly(3,4-ethelenedioxythiophene) * |
| ZnO nanocomposite and photocatalytic activity》.《Nanoscale Research Letters》.2014,第9卷(第1期),(89)1-8. * |
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