CN108963001A - A kind of method of located growth perovskite thin film array - Google Patents
A kind of method of located growth perovskite thin film array Download PDFInfo
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- 239000003795 chemical substances by application Substances 0.000 claims description 2
- OJZNZOXALZKPEA-UHFFFAOYSA-N chloro-methyl-diphenylsilane Chemical group C=1C=CC=CC=1[Si](Cl)(C)C1=CC=CC=C1 OJZNZOXALZKPEA-UHFFFAOYSA-N 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 229960004756 ethanol Drugs 0.000 claims description 2
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
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- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 2
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
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- 239000010408 film Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
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- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 description 1
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- H01L31/02—Details
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Abstract
The invention discloses a kind of methods of located growth perovskite thin film array, it is after carrying out hydrophobicity processing to the surface of silicon with insulating layer, pass through uv-exposure photoetching technique again, positioning needs to grow the region of perovskite thin film array on substrate, form the photoresist layer with array window, then substrate is bombarded using oxygen plasma, makes window area hydrophiling；Photoresist is finally removed, spin coating perovskite precursor solution is simultaneously annealed, that is, forms perovskite thin film array.Present invention combination uv-exposure photoetching technique, selectivity realize the hydrophilicity-imparting treatment of substrate surface, provide a kind of very simple and feasible mode for the located growth of membrane array, provide new thinking for the preparation of photosensor arrays.
Description
Technical field
The invention belongs to the technical fields of perovskite thin film growth, and in particular to a kind of located growth perovskite thin film array
Method.
Background technique
Photodetector is the semiconductor devices for converting optical signal into electric signal, in daily life, national economy and army
Thing field plays the role of particularly important.More pixel sensor arrays based on single photodetector, due to can be real
The photodetection of existing large area, multiple types, effectively improves that single photodetector investigative range is small, lacking of having a single function
Point can be applied to the fields such as image sensing, real time imagery, thus has and be more widely applied.
Traditional sensors array is to realize the positioning of pixel, it usually needs experience multiple bearing photoetching process is realized
Selective deposition, etching of semiconductor material etc., or pixel is positioned to realize semiconductor material by photoetching process
Located growth.
In recent years, perovskite is as a kind of emerging material, since absorption coefficient is high, band gap is adjustable, charge propagation distance
Long and high photoelectric conversion efficiency feature, is widely used in field of photoelectric devices.Institutes Of Technology Of Nanjing Zeng Haibo professor
(Adv.Mater., 2016,28,4861) just once by way of printing, realizes few inorganic perovskite material of layer in flexible substrate
CsPbBr3The preparation of high-performance optical electric explorer, 19 μm of the detector rise time, 24 μm of fall time, on-off ratio are up to 104
And good repeatable and stability.HeFei University of Technology's Luo Lin care and education of infants, which awards also once to realize by spin-coating method, to be based on
FA0.85Cs0.15PbI3Perovskite thin film from driving photodetector preparation (Adv.Opt.Mater., 2017,5,
1700654)。
However since the characteristic of perovskite material itself, growth cannot contact water equal solvent after completing, this to pass
Semiconductor technology of system such as uv-exposure photoetching etc., it is impossible to be used in the growth of perovskite array structure, this largely upper limit
Perovskite material has been made in the application in photodetector array field.
2016, professor Fan Zhiyong was that template is realized by two-step method with 1024 pixels using anodised aluminium
The MaPbI of point3Three-dimension sensor array prepares (Adv.Mater., 2016,28,9713), has successfully inquired into perovskite array work
For the application of imaging sensor.However the preparation process of complicated anodic oxidation aluminium formwork can not be ignored, and perovskite array
It is not corresponded with pixel, therefore the controllability of sensor array growth is still up for further being promoted.So far, base
In the one-step method controllable growth of the array structure of perovskite thin film, still it is rarely reported.
Summary of the invention
On basis of the existing technology, the present invention is directed to construct a kind of simple, located growth perovskite thin film
The method of array, the technical problem to be solved is that realize perovskite thin film array by substrate surface selectivity hydrophilic treated
Located growth, this has great significance in the preparation field of photosensor arrays.
The present invention solves technical problem, adopts the following technical scheme that
The method of located growth perovskite thin film array of the present invention, it is characterized in that: the list of insulating layer is covered with surface
Crystal silicon is substrate, to substrate carry out hydrophobicity processing after, on the insulating layer spin coating photoresist and pass through uv-exposure photoetching
Technology, positioning needs to grow the region of perovskite thin film array on the insulating layer, forms the photoresist with array window
Layer；Then hydrophily processing is carried out to array window with oxygen plasma, makes array window area hydrophiling；Photoresist is removed again
Layer, spin coating perovskite precursor solution is last annealed, i.e., realizes the growth of perovskite thin film at array window, obtain calcium
Titanium ore membrane array.
Further: the perovskite thin film is FAxCs1-xPbI3(0≤x≤1)、CsPbBr3、CsBi3I10Or its ion
The product of doping；The precursor solution concentration is 0.5-2mol/L.
Further: the monocrystalline silicon is single-sided polishing, and the surface roughness of burnishing surface is not more than 1nm；The insulating layer
For SiO2Insulating layer, Si3N4Insulating layer, HfO2Insulating layer or Al2O3The resistivity of insulating layer, the insulating layer is not less than 1 × 103
Ω cm, with a thickness of 100-500nm.
Further: the hydrophobicity processing is to carry out deep clean to the substrate surface；Or the hydrophobicity processing
It is after carrying out deep clean to the surface of the substrate, to be coated silane coupling agent and carry out surface modification treatment.
Further: the deep clean is first to be impregnated, be ultrasonically treated to remove and have to substrate with organic solvent
Machine pollutant, then the pollutant of physical absorption is removed with deionized water ultrasound, it is finally rinsed again with deionized water, drying；Or:
The deep clean is first to be impregnated, be ultrasonically treated to remove each pollutant to substrate with electronic cleaning agent, is then used again
Deionized water is rinsed, is dried up.It is described coating silane coupling agent be by substrate volumetric concentration be 0.1%-10% it is silane coupled
In the toluene or ethanol solution of agent, after soaking at room temperature 10min, it is heated to 60-150 DEG C of holding 30min or more.
Yet further: the silane coupling agent is diphenyl methyl chloro silane or octadecyl trichlorosilane alkane；It is described to have
Solvent is chloroform, acetone or dehydrated alcohol；The electronic cleaning agent is DZ-1 or DZ-2.
Further: the array window is formed by spin coating photoresist, uv-exposure photoetching and developing process；It is described
The thickness of photoresist is not less than 1 μm；The size of each window is not less than 50 μm * 50 μm, and the minimum range between adjacent window apertures is not small
In window size.
Further: the hydrophily processing is passed through using plasma washing machine or reactive ion etching system
Oxygen plasma bombards array window area, forms clean surface, and form the hydroxyl of suspension.Further: it is described it is equal from
The operating condition of daughter cleaning machine are as follows: oxygen flow 2.5sccm, sputtering power 18W sputter 50min；The reactive ion is carved
The operating condition of erosion system are as follows: oxygen flow 20sccm, sputtering power 50W sputter 5min.
Further: the annealing is the 10min that anneals under conditions of 135 DEG C.
Compared with the prior art, the beneficial effects of the present invention are embodied in:
1, the present invention is successfully realized calcium titanium in conjunction with uv-exposure photoetching technique by simple hydrophobic and hydrophilic treated
The located growth of mine membrane array provides a kind of new thinking for the preparation of the photosensor arrays based on it.
2, the present invention has good compatibility with existing silicon semiconductor technique, it is easy to accomplish device is in existing integrated circuit
It is integrated on chip.
Detailed description of the invention
Fig. 1 is the flow chart of located growth perovskite thin film array of the present invention, in which: 1 is monocrystalline silicon, and 2 be insulating layer, 3
It is oxygen plasma for the photoresist layer with array window, 4,5 be hydrophilic region, and 6 be perovskite thin film array.
Fig. 2 is that the SEM for 5 × 5 array structures that the size of located growth in the embodiment of the present invention 1 is 300 μm of 300 μ m shines
Piece.
Fig. 3 is the step instrument horizontal sweep map of the array structure of located growth in the embodiment of the present invention 1.
Fig. 4 is the SEM for 10 × 10 array structures that the size of located growth in the embodiment of the present invention 2 is 100 μm of 100 μ m
Photo.
Fig. 5 is the step instrument horizontal sweep map of the array structure of located growth in the embodiment of the present invention 2.
Specific embodiment
It elaborates with reference to the accompanying drawing to the embodiment of the present invention, following embodiments are being with technical solution of the present invention
Under the premise of implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to
Following embodiments.
Embodiment 1
Referring to Fig. 1, perovskite array of the invention is that the monocrystalline silicon 1 of insulating layer 2 is covered with surface is substrate, to substrate
After carrying out hydrophobicity processing, spin coating photoresist and is formed by uv-exposure photoetching technique there is array window on the insulating layer
Photoresist layer 3；Then hydrophily processing is carried out to array window with oxygen plasma 4, makes to form hydrophily area at array window
Domain 5；Photoresist layer is removed again, and spin coating perovskite precursor solution is last annealed, i.e., realizes that perovskite is thin at array window
The growth of film obtains perovskite thin film array 6.Specific step is as follows:
(1) surface is taken to be covered with 300nm SiO2Insulating layer (resistivity 1 × 103Ω cm) monocrystalline silicon (single-sided polishing,
The surface roughness of burnishing surface is not more than 1nm) it is used as substrate, following hydrophobicity processing is carried out to substrate: using deionized water first
Substrate is rinsed, substrate is then placed on immersion 30min, ultrasound 10min in electronic cleaning agent DZ-1；Then rinsed with deionized water
5min；30min, ultrasound 10min are impregnated in electronic cleaning agent DZ-2 again；After finally rinsing 5min with deionized water again, nitrogen
Drying.
(2) after hydrophily processing, (spincoating conditions: low speed 600rpm revolves spin coating AR-5350 positive photoresist photoresist on the insulating layer
Apply 9s, high speed 3000rpm spin coating 30s, about 1 μm of photoresist thickness), it is then (thin according to required perovskite using specific mask plate
The size of membrane array is determined) after uv-exposure, development obtains the photoresist layer with array window.
(3) hydrophily processing is carried out to array window with oxygen plasma, makes to form hydrophilic region at array window: by light
Substrate after quarter is put into plasma washing machine (PDC-32G), after cavity vacuumizes, is passed through the high pure oxygen of purity 99.5%
Gas, control oxygen flow are 2.5sccm, are bombarded 50 minutes after stablizing using high-power mode (sputtering power 18W).
(4) photoresist layer is removed, direct spin-coating method spin coating FA is utilized0.85Cs0.15PbI3Precursor solution, then again in sky
FA is realized in 135 DEG C short annealing 10 minutes in gas that is, at array window0.85Cs0.15PbI3The growth of film obtains
FA0.85Cs0.15PbI3Membrane array.
Specifically, FA0.85Cs0.15PbI3Precursor solution the preparation method is as follows: taking 0.154 gram of carbonamidine iodine, 0.026 gram
Cesium iodide, 0.462 gram of lead iodide mixing are put into vial, and 800 μ L NN- dimethylformamides, 200 μ L dimethyl sulfoxides are added, surpass
Sound dissolution, is then placed on 75 DEG C of magnetic agitation 10min on warm table, obtains the FA that concentration is 1mol/L0.85Cs0.15PbI3Forerunner
Liquid solution.
The present embodiment size obtained be 300 μm of 300 μ m 5 × 5 array structures SEM photograph as shown in Fig. 2, from
It can be seen that each pixel all homoepitaxials have perovskite thin film in figure, and there is no the life of perovskite thin film except pixel
It is long, show the located growth for being successfully realized perovskite thin film.
Fig. 3 show the step instrument horizontal sweep map of the array structure of located growth in the present embodiment.It can be with from figure
Find out, about 1.6 μm of the thickness of perovskite thin film or so, the thickness uniformity of each pixel is preferable.
Embodiment 2
The method of the located growth of the present embodiment is same as Example 1, and difference is only that in the present embodiment that preparing is picture
10 × 10 array structures of 100 μm of 100 μ m of vegetarian refreshments size.
The SEM photograph of the present embodiment array structure obtained as shown in figure 4, from figure can each pixel it is all uniform
Growth has perovskite thin film, and does not have the growth of perovskite thin film except pixel, shows to be successfully realized perovskite thin film
Located growth.
Fig. 5 show the step instrument horizontal sweep map of the array structure of located growth in the present embodiment.It can be with from figure
Find out, thickness about 600nm of perovskite thin film or so.With the reduction of pixel spot size, hydrophily treatment effect is declined slightly,
The thickness of product perovskite thin film reduces, but still has preferable the thickness uniformity between each pixel.
The above is only exemplary embodiment of the present invention, are not intended to limit the invention, all in spirit of the invention
With any modifications, equivalent replacements, and improvements made within principle etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of method of located growth perovskite thin film array, it is characterised in that: be covered with the monocrystalline silicon of insulating layer with surface
For substrate, after carrying out hydrophobicity processing to substrate, the spin coating photoresist and by uv-exposure photoetching technique on the insulating layer,
Positioning needs to grow the region of perovskite thin film array on the insulating layer, forms the photoresist layer with array window；So
Hydrophily processing is carried out to array window with oxygen plasma afterwards, makes array window area hydrophiling；Photoresist layer is removed again, is revolved
Perovskite precursor solution is applied, it is last annealed, i.e., the growth of perovskite thin film is realized at array window, and it is thin to obtain perovskite
Membrane array.
2. the method for located growth perovskite thin film array according to claim 1, it is characterised in that: the perovskite is thin
Film is FAxCs1-xPbI3(0≤x≤1)、CsPbBr3、CsBi3I10Or the product of its ion doping；
The precursor solution concentration is 0.5-2mol/L.
3. the method for located growth perovskite thin film array according to claim 1, it is characterised in that:
The monocrystalline silicon is single-sided polishing, and the surface roughness of burnishing surface is not more than 1nm；
The insulating layer is SiO2Insulating layer, Si3N4Insulating layer, HfO2Insulating layer or Al2O3Insulating layer；
The resistivity of the insulating layer is not less than 1 × 103Ω cm, with a thickness of 100-500nm.
4. the method for located growth perovskite thin film array according to claim 1, it is characterised in that:
The hydrophobicity processing is to carry out deep clean to the substrate surface；
Or: the hydrophobicity processing is after carrying out deep clean to the surface of the substrate, to be coated silane coupling agent carry out table
Face modification.
5. the method for located growth perovskite thin film array according to claim 4, it is characterised in that:
The deep clean is first to be impregnated, be ultrasonically treated to remove removal organic polluter to substrate with organic solvent, then spent
Ionized water ultrasound is finally rinsed with deionized water, drying again with removing the pollutant of physical absorption；Or: the deep clean is
First substrate is impregnated with electronic cleaning agent, is ultrasonically treated to remove each pollutant, then rinsed, blown with deionized water again
It is dry；
The coating silane coupling agent is the toluene or ethyl alcohol of the silane coupling agent by substrate in volumetric concentration for 0.1%-10%
In solution, after soaking at room temperature 10min, it is heated to 60-150 DEG C of holding 30min or more.
6. the method for located growth perovskite thin film array according to claim 5, it is characterised in that: described silane coupled
Agent is diphenyl methyl chloro silane or octadecyl trichlorosilane alkane；The organic solvent is chloroform, acetone or dehydrated alcohol；
The electronic cleaning agent is DZ-1 or DZ-2.
7. the method for located growth perovskite thin film array according to claim 1, it is characterised in that: the array window
It is formed by spin coating photoresist, uv-exposure photoetching and developing process；
The thickness of the photoresist is not less than 1 μm；
The size of each window is not less than 50 μm * 50 μm, and the minimum range between adjacent window apertures is not less than window size.
8. the method for located growth perovskite thin film array according to claim 1, it is characterised in that: at the hydrophily
Reason is to bombard array window area, shape by oxygen plasma using plasma washing machine or reactive ion etching system
At clean surface, and form the hydroxyl of suspension；
The operating condition of the plasma washing machine are as follows: oxygen flow 2.5sccm, sputtering power 18W sputter 50min；
The operating condition of the reactive ion etching system are as follows: oxygen flow 20sccm, sputtering power 50W sputter 5min.
9. the method for located growth perovskite thin film array according to claim 1, it is characterised in that: it is described annealing be
Anneal 10min under conditions of 135 DEG C.
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| CN110294455A (en) * | 2019-06-26 | 2019-10-01 | 上海大学 | Functional material located growth method |
| CN110482530A (en) * | 2019-09-04 | 2019-11-22 | 北京华碳元芯电子科技有限责任公司 | A method of preparing patterned carbon nanotube film |
| CN110942981A (en) * | 2019-12-10 | 2020-03-31 | 上海华力微电子有限公司 | Gluing method and semiconductor structure |
| CN111490144A (en) * | 2019-01-28 | 2020-08-04 | 致晶科技（北京）有限公司 | Preparation method of quantum dot patterned film and patterned film |
| CN111952463A (en) * | 2020-08-26 | 2020-11-17 | 合肥工业大学 | Preparation method of large-area perovskite nanowire array |
| CN112279214A (en) * | 2019-07-25 | 2021-01-29 | 首都师范大学 | Method for preparing concentric ring structure on surface of perovskite thin film |
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| CN111490144B (en) * | 2019-01-28 | 2024-02-02 | 致晶科技（北京）有限公司 | Preparation method of quantum dot patterning film and patterning film |
| CN110294455A (en) * | 2019-06-26 | 2019-10-01 | 上海大学 | Functional material located growth method |
| CN112279214A (en) * | 2019-07-25 | 2021-01-29 | 首都师范大学 | Method for preparing concentric ring structure on surface of perovskite thin film |
| CN112279214B (en) * | 2019-07-25 | 2023-12-22 | 首都师范大学 | Method for preparing concentric ring structure on perovskite film surface |
| CN110482530A (en) * | 2019-09-04 | 2019-11-22 | 北京华碳元芯电子科技有限责任公司 | A method of preparing patterned carbon nanotube film |
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| CN111952463A (en) * | 2020-08-26 | 2020-11-17 | 合肥工业大学 | Preparation method of large-area perovskite nanowire array |
| CN111952463B (en) * | 2020-08-26 | 2023-04-07 | 合肥工业大学 | Preparation method of large-area perovskite nanowire array |
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