CN105355795A - Photoelectric detector array manufacture method based on conjugated polymer nanometer crystal lamination type self-assembling function film - Google Patents

Photoelectric detector array manufacture method based on conjugated polymer nanometer crystal lamination type self-assembling function film Download PDF

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CN105355795A
CN105355795A CN201510862765.0A CN201510862765A CN105355795A CN 105355795 A CN105355795 A CN 105355795A CN 201510862765 A CN201510862765 A CN 201510862765A CN 105355795 A CN105355795 A CN 105355795A
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film
substrate
conjugated polymer
self
photoelectric detector
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张遒姝
彭倍
李辉
孙江涛
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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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
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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Abstract

The invention discloses a photoelectric detector array manufacture method based on a conjugated polymer nanometer crystal lamination type self-assembling function film, comprising steps of adopting an optical etching technology to transfer a photoelectric detector array anode pattern to an ITO film on the glass substrate surface, performing surface modification on the ITO film forming the anode pattern to enable the ITO film to carry negative electricity, alternatively putting the substrate into a conjugated polymer dilution solution and a nanometer crystal dilution solution with negative electricity for immersing, repeating the above steps until the self-assembling film deposited on the surface of the substrate ITO film achieves the appropriate thickness, and adopting the thermal evaporation technology to continuously deposit LiF and Al film on the surface of the self-assembling film to obtain the photoelectric detector array of the self-assembling film based on the conjugated polymer nanometer crystal lamination type. The photoelectric detector array is low in the array, can effectively optimize or regulate the performance of the photoelectric detector through changing the self-assembling film component material and lamination number and can obtain the high performance member.

Description

Based on the photodetector array manufacture method of conjugated polymer-nanocrystalline laminated type self-assembly function film
Technical field
The invention belongs to nanometer technology and optoelectronic device technology field, be specifically related to a kind of manufacture method of the photodetector array based on conjugated polymer-nanocrystalline laminated type self-assembly function film.
Background technology
Traditional photodetector makes with inorganic semiconductor materials such as CdSe, CdTe, PbS, PbSe.Inorganic semiconductor material has highly stable optics and electric property, and processing technology is ripe.But the limitation of inorganic semiconductor material also annoyings academia and industrial quarters always.First the material category being it is very limited, and various performance number is in a discrete distribution state.Although doping can revise the performance of inorganic semiconductor material effectively, doping needs high temperature and quite complicated technique, cost intensive.And under the trend that electronic devices and components are day by day microminiaturized, the nanometer technology based on inorganic semiconductor will meet with the bottleneck of manufacturing dimension restriction.In addition, inorganic semiconductor material is hard, lacks flexible, is difficult to be applied to curved surface or ductility requires high occasion.
In order to overcome the limitation of inorganic semiconductor material in performance and manufacturing process etc., some new nanometer technologies are arisen at the historic moment, and the laminated type nanometer self-assembly thin film technique of " from bottom to top " is one of them.This nanometer technology is by the electrostatic interaction of size between the charged group element material of Nano grade, make " constructing part " polymer molecule or nano particle with the growth ladder of every layer of about 1nm successively alternating sorbent form film at substrate surface, finally realize predetermined micro-/ nano functional structure.Laminated type nanometer self-assembly technology is build the function film meeting particular characteristic requirement to provide the very large degree of freedom, because group element material, layer number and laminated layer sequence can carry out changing or adjusting as required.Another outstanding advantage of this technology is simple and easy to do and with low cost.Except silicon and the glass substrate of routine, laminated type nanometer self-assembly film can also be built in the good plastic of pliability, thus can be applicable to some special applied environment, such as curved surfaces.The application of laminated type nanometer self-assembly technology on opto-electronic device has obvious advantage, because it can not only accurately control the structure of film, composition and thickness from molecule aspect, the device with hole transport polymer layer, photosensitive layer, electronics transport polymer layer alternating laminated structure also may be realized.At present, laminated type nanometer self-assembly film has been applied to optoelectronic switch, electrochromic device, solar cell, fuel cell, light-emitting diode, but this new nanometer technology application on photodetector is few.
Conjugated polymer is novel organic semiconducting materials, can be used as photodetector active layer.Photodetector based on conjugated polymer has lightweight, flexible shape, the advantage such as with low cost, is up-and-coming New Generation Optical electric explorer.And inorganic nano-crystal (also referred to as quantum dot) is the low dimensional semiconductor material had a extensive future, its special feature is, because the effect of quantum confinement effect, it absorbs and emitted energy depends on size significantly, and the performance shown is between molecule and main body.Because spectral quality depends on size, three-dimensional limits to the high-quantum efficiency and potential carrier multiplication that cause, to be nanocrystallinely used in photodetector as sensitising agent.The nano composite material that formed of being combined with conjugatd polymers by inorganic semiconductor nano particle, because combine electricity and the optical property of organic semiconductor and inorganic semiconductor, very likely presents unique optical physics, photochemistry and chemical property.Composite material semiconductor nano being doped in the formation of conjugated polymer matrix is applied to photodetector, demonstrates excellent device performance.Such as, based on poly [2-methoxy-5-(2'-ethylhexyloxy)-1,4-phenylenevinylene] the photodetector external quantum efficiency of (MEH-PPV)/PbSe Nanocrystalline Composite Films reaches as high as 150% (-8V, 510nm, MEH-PPV content is 95%w, nanocrystallinely be of a size of 8nm), its active layer is formed by the mixed solution that spin coating MEH-PPV and PbSe is nanocrystalline.Although use conventional solution mixing, spin coating can produce high performance device, the thickness of film is difficult to control or reappear, and also can the material of large losses in the course of processing.
Summary of the invention
For overcoming the shortcoming and defect that prior art exists, the invention provides a kind of manufacture method of the photodetector array based on conjugated polymer-nanocrystalline laminated type self-assembly function film.
Technical scheme of the present invention is as follows:
Based on a manufacture method for the photodetector array of conjugated polymer-nanocrystalline laminated type self-assembly function film, comprise the following steps:
A: the formation of photodetector anode-array pattern on substrate ito thin film
1) spin coating technique is adopted to be coated in by photoresist on cleaned glass-ITO substrate equably;
2) photoetching technique is adopted to transfer on the ito thin film of glass substrate surface by photodetector array anode pattern;
B: the preparation of conjugated polymer-nanocrystalline laminated type self-assembly function film
3) by step 2) the ITO substrate defining anode pattern of gained successively puts into acetone and isopropyl alcohol, with ultrasonic washing instrument cleaning, finally dries up substrate by nitrogen gun;
4) to through step 3) ito thin film of substrate surface after process carries out surface modification makes it electronegative;
5) by through step 4) substrate after the process conjugated polymer dilute solution of putting into positively charged soaks a period of time, and cleaning after taking out, removes the material of surface porosity absorption;
6) by through step 5) substrate after process puts into another electronegative nanocrystalline dilute solution and soaks, clean after taking-up again;
7) circulation carry out step 5) and step 6) until the conjugated polymer-nanocrystalline laminated type self-assembly film of substrate ito thin film surface deposition reaches suitable thickness (50nm-200nm);
C: the formation of photodetector array cathode construction
8) thermal evaporation techniques is adopted in step 7) the self-assembly film surface that obtains deposition LiF film (5A);
9) thermal evaporation techniques is adopted in step 8) LiF film surface depositing Al film (200nm) that obtains.
Compared with prior art, beneficial effect of the present invention is:
Photodetector array based on conjugated polymer-nanocrystalline laminated type self-assembly function film of the present invention can be built on larger area, lightweight and thin, and pliability is good, with low cost.But also by changing the character of group element material, laminated layer sequence, layer number and film preparation condition free ground amendment self-assembly film, thus can effectively optimize or regulate the performance of photodetector, obtain high performance device.
Invention has been following method to improve:
Adoptable nanocrystalline material has: CdS, CdSe, CdTe, PbS, PbSe, InSb, and nanocrystalline diameter is 4nm-8nm, and these semiconductor nanos have high electron mobility, and can overcome the charge transport restriction that organic material causes.Spendable conjugated polymer comprises poly (p-phenylene) (PPP), poly (p-phenylenevinylene) (PPV), poly (p-phenyleneethynylene) (PPE), the electrical and optical property of these polymer can mate with inorganic nano-crystal the photoelectron performance producing excellence well.By selecting suitable conjugated polymer material and nanocrystalline material and size, can be optimized photoelectric detector performance or regulate.
Accompanying drawing explanation
Fig. 1 is the plastic mask schematic diagram for etching ito thin film.
Fig. 2 is the forming process schematic diagram of conjugated polymer-nanocrystalline laminated type self-assembly function film.
Fig. 3 is shadow mask (shadowmask) schematic diagram for depositing LiF and Al film.
Fig. 4 is the photodetector device structural representation based on conjugated polymer-nanocrystalline laminated type self-assembly function film of the present invention.
Fig. 5 is the photodetector array schematic diagram based on conjugated polymer-nanocrystalline laminated type self-assembly function film.
Wherein: in Fig. 4 and Fig. 5: 1-conjugated polymer-nanocrystalline laminated type self-assembly function film; 2-ITO film; 3-Al film; 4-LiF film; 5-glass.
Fig. 6 is the photodetector device I-E characteristic based on PPV-CdSe nanocrystalline laminated type self-assembly function film.Test condition is power density 68 μ W/cm 2the illumination of 510nm monochromator.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail, but embodiments of the present invention are not limited thereto.
Embodiment
Manufacture process based on the photodetector array of conjugated polymer PPV-CdSe nanocrystalline laminated type self-assembly function film:
A: the formation of photodetector anode-array pattern on substrate ito thin film
1) spin coating technique is adopted photoresist to be coated in equably the cleaned glass 5-ITO substrate (Delta'sTechnologiesLimited being of a size of 25 × 25 × 1.1mm, Stillwater, MN, USA) on, ITO substrate surface resistance is 5 ~ 15 Ω/sq;
2) adopt photoetching technique photodetector array anode pattern to be transferred on the ito thin film of glass 5 substrate surface, the corrosive agent of etching ITO is hydrochloric acid (HCl), for etching the plastic mask of ITO as shown in Figure 1;
The preparation of B:PPV-CdSe nanocrystalline laminated type self-assembly function film 1
CdS semiconductor e is nanocrystalline has high electron mobility, and the charge transport restriction that organic material causes can be overcome, and the electrical and optical property of conjugated polymer poly (p-phenylenevinylene) (PPV) can mate with inorganic nano-crystal the photoelectron performance producing excellence well.Amine is introduced PPV side chain and functional modification is carried out to it, obtain the PPV-NH of positively charged 2, introduce pentafluorophenyl group ester side chain and then obtain electronegative PPV-COOR; At CdSe (particle diameter 4nm) nanocrystal surface deposition carboxylate, then obtained the electronegative CdSe nanocrystalline (CdSe-COOR) of surface coverage pentafluorophenyl group ester by activation.The preparation process of PPV-CdSe nanocrystalline laminated type self-assembly function film 1 is as follows:
3) by step 2) ito thin film 2 defining anode pattern of gained successively puts into acetone and isopropyl alcohol together with glass 5 substrate, with ultrasonic washing instrument cleaning, finally dries up substrate by nitrogen gun;
4) will through step 3) ito thin film 2 after process together with glass 5 substrate at N 23-aminopropyl triethoxysilane (APTES) toluene solution (temperature 90 DEG C that weight fraction is 5% is immersed under environment, the 1 hour time), then clean with toluene and dry up by nitrogen gun, namely obtaining with the ito thin film 2 of the positively charged of amino-functionalization modification;
5) by step 4) ito thin film 2 of surface band positive electricity that obtains at room temperature immerses together with glass 5 substrate the CH that concentration is the PPV-COOR of 1mg/mL 2cl 2solution 20 minutes, then uses CH 2cl 2thoroughly clean with ethanol, finally dry up with nitrogen, namely define ground floor PPV, through step 4 on ito thin film 2 surface) and step 5) process after ito thin film 2 surface band negative electricity (Fig. 2-1);
6) by step 5) obtain through ground floor PPV modify ito thin film 2 at room temperature immerse together with glass 5 substrate the PPV-NH that concentration is 1mg/mL 2cH 2cl 2solution 20 minutes, uses CH after deposition 2cl 2thoroughly clean with ethanol, finally dry up (Fig. 2-2 and Fig. 2-3) with nitrogen;
7) by step 6) ito thin film 2 that deposited second layer PPV that obtains at room temperature immerses together with glass 5 substrate the CdSe-COOR ethanolic solution 20 minutes that concentration is 1mg/mL, uses CH after deposition 2cl 2thoroughly clean with ethanol, finally dry up (Fig. 2-4 and Fig. 2-5) with nitrogen;
8) circulation carry out step 6) and step 7) until the PPV-CdSe nanocrystalline laminated type self-assembly film 1 of substrate ito thin film 2 surface deposition reaches suitable thickness (50nm-200nm), Fig. 2-6 to Fig. 2-9 is the forming process of second group of nanocrystalline bilayer of PPV-CdSe;
C: the formation of photodetector array cathode construction
9) thermal evaporation techniques is adopted in step 8) the surperficial successive sedimentation LiF (5A) 4 of self-assembly film 1 that obtains and Al (200nm) film 3, for depositing the shadow mask of LiF4 and Al film 3 as shown in Figure 3, Fig. 4 is the photodetector device structural representation based on conjugated polymer-nanocrystalline laminated type self-assembly function film 1, and the effective area of each photodetector device that anode and negative electrode overlap produce is 9mm 2, after completing LiF4 and Al film 3 deposition, namely obtain the photodetector array (Fig. 5) based on PPV-CdSe nanocrystalline laminated type self-assembly function film 1.
Follow-up test
With PPV-CdSe nanocrystalline laminated type self-assembly function film for the simple photodetector device of active layer manufacture, apparatus structure is ITO/ (PPV – CdSe) 18/ Al, wherein device active layer is formed by the nanocrystalline bilayer of deposition 18 groups of PPV-CdSe, and thickness is about 90nm, and negative electrode Al film thickness is 200nm, and device effective area is 9mm 2.The I-E characteristic of device adopts the picoammeter (Keithley6487) of gpib interface (NationalInstrument) remote control to measure in atmosphere, measurement result as shown in Figure 6, is less than 10 at the reverse biased scope dark current of 0>V>-8V -7a, 1-2 the order of magnitude lower than photoelectric current, external quantum efficiency is 80% as calculated.Test result shows, and PPV-CdSe nanocrystalline laminated type self-assembly function film can be used for manufacturing high-performance optical electric explorer.
Above-described embodiment is one of embodiment of the present invention, and other is any does not deviate from the improvement or conversion that the technology of the present invention principle does, within the protection range that all should be included in claims of the present invention.

Claims (1)

1., based on the photodetector array manufacture method of conjugated polymer-nanocrystalline laminated type self-assembly function film, it is characterized in that, comprise the following steps:
A: the formation of photodetector anode-array pattern on substrate ito thin film;
1) spin coating technique is adopted to be coated in by photoresist on cleaned glass-ITO substrate equably;
2) photoetching technique is adopted to transfer on the ito thin film of glass substrate surface by photodetector array anode pattern;
B: the preparation of conjugated polymer-nanocrystalline laminated type self-assembly function film;
3) by step 2) the ITO substrate defining anode pattern of gained successively puts into acetone and isopropyl alcohol, with ultrasonic washing instrument cleaning, finally dries up substrate by nitrogen gun;
4) to through step 3) ito thin film of substrate surface after process carries out surface modification makes it electronegative;
5) by through step 4) substrate after the process conjugated polymer dilute solution of putting into positively charged soaks a period of time, and cleaning after taking out, removes the material of surface porosity absorption;
6) by through step 5) substrate after process puts into another electronegative nanocrystalline dilute solution and soaks, clean after taking-up again;
7) circulation carry out step 5) and step 6) until the conjugated polymer-nanocrystalline laminated type self-assembly film of substrate ito thin film surface deposition reaches thickness 50nm-200nm;
C: the formation of photodetector array cathode construction;
8) thermal evaporation techniques is adopted in step 7) the self-assembly film surface that obtains deposition LiF film;
9) thermal evaporation techniques is adopted in step 8) the LiF film surface depositing Al film 200nm that obtains.
CN201510862765.0A 2015-12-01 2015-12-01 Photoelectric detector array manufacture method based on conjugated polymer nanometer crystal lamination type self-assembling function film Pending CN105355795A (en)

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CN103262281A (en) * 2011-02-14 2013-08-21 南佛罗里达大学 Organic photovoltaic array and method of manufacture
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Publication number Priority date Publication date Assignee Title
US20050098204A1 (en) * 2003-05-21 2005-05-12 Nanosolar, Inc. Photovoltaic devices fabricated from nanostructured template
CN101473463A (en) * 2006-06-22 2009-07-01 依索沃尔塔股份公司 Method for producing a layer containing inorganic semiconductor particles, and components comprising said layer
CN101976729A (en) * 2010-09-30 2011-02-16 昆明物理研究所 Plane-configured organic infrared or ultraviolet photovoltaic semiconductor detector
CN103262281A (en) * 2011-02-14 2013-08-21 南佛罗里达大学 Organic photovoltaic array and method of manufacture
CN104821374A (en) * 2015-03-12 2015-08-05 华南理工大学 Preparation method of organic optoelectronic device cathode interface layer based on conjugated polyelectrolyte and application thereof

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ZIQI LIANG ET AL.: "《Covalent Layer-by-Layer Assembly of Conjugated Polymers and CdSe Nanoparticles: Multilayer Structure and Photovoltaic Properties》", 《ADVANCED FUNCTIONAL MATERIALS》 *

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Application publication date: 20160224