CN109742242A - A kind of wide spectrum nano-array detector and preparation method thereof - Google Patents
A kind of wide spectrum nano-array detector and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of wide spectrum nano-array detectors, including silicon oxide substrate, ZnO nano column periodic array structure is arranged in the surface of silicon oxide substrate, perovskite nano-pillar periodic array structure is arranged in ZnO nano column periodic array body structure surface, ZnO nano column and perovskite nano-pillar consistency from top to bottom constitute axial hetero-junctions cylinder, transparent conductive film is arranged in the surface of silicon oxide substrate and the surface of axial hetero-junctions cylinder, and the surface setting metal grid lines electrode positioned at the transparent conductive film of ZnO nano column periodic array structure two sides drives as conductive electrode for external circuit.The invention also discloses a kind of preparation methods of wide spectrum nano-array detector.The present invention expands the spectral response range of ZnO using perovskite and the periodic array of nano-pillar, and the response of higher visible spectrum is generated on the basis of not losing ZnO ultraviolet spectra and responding.
Description
Technical field
The present invention relates to a kind of spectral detectors and preparation method thereof, detect more particularly, to a kind of wide spectrum nano-array
Device and preparation method thereof.
Background technique
Prominent as third generation semiconductor represents, and zinc oxide (ZnO) is due to its excellent comprehensive performance, good stabilization
It property and is had a wide range of applications the features such as convenient for preparing in fields such as optics, electronics, magnetics, electrochemistry.Room temperature
The direct band gap of lower ZnO is 3.37eV, and it is a kind of efficient short-wavelength light electronic material that exciton bind energy, which is up to 60meV,.ZnO
Good electron transport property makes it also have huge application potential in photovoltaic and photocatalysis field application prospect.
But its broad-band gap limits its absorption to the visible light for accounting for solar energy about 43%.The low efficiency of light energy utilization greatly limits
Practical application of the ZnO as photoelectric material is made.Various countries researcher makes its optical response range from purple using the trial of a variety of methods
Wave section extends to visible-range, improves the utilization rate of material light.Deng etc. modifies the surface ZnO by Ag, can by Ag base
Light-exposed plasma resonance peak makes ZnO have preferable absorption (Deng Q, Duan X, Ng D H L, et al.ACS to visible light
Applied Materials&Interfaces,2012,4(11):6030–6037.);Cho etc. utilizes compound three of ZnO/ZnSe
Wiener rice rod structure (Cho S, Jang J W, Kim J, et al.Langmuir, 2011,27 (16): 10243-10250.), changes
The good photoelectric respone of material under visible light;The patent of invention ZL201210370194.5 of Tsinghua University, which provides one kind, to be had
The ZnO material and preparation method thereof of oxygen defect type, improves the response of the visible region of material.CH3NH3PbX3(X=Br, I) is
One kind has the hybrid inorganic-organic semiconductor material of perovskite crystal structure type, has the biggish absorption coefficient of light and electricity
Son-hole-diffusion length.Wherein CH3NH3PbI3Direct band gap with 1.55ev, energy absorbing wavelength are less than the photon of 800nm,
Visible light part corresponding to solar spectrum.
Summary of the invention
It is an object of the present invention to provide a kind of wide spectrum nano-array detectors, utilize perovskite and the week of nano-pillar
Phase array expand ZnO spectral response range, do not lose ZnO ultraviolet spectra (300~450nm) response on the basis of generate compared with
The response of high visible spectrum (450~800nm), while higher responsiveness is realized using ZnO excellent carrier transport spy.
It is a further object to provide a kind of preparation methods of wide spectrum nano-array detector.
Technical solution of the present invention is as follows: a kind of wide spectrum nano-array detector, including silicon oxide substrate, the silica
ZnO nano column periodic array structure is arranged in the surface of substrate, and the ZnO nano column periodic array body structure surface setting perovskite is received
Rice column periodic array structure, the ZnO nano column and the perovskite nano-pillar consistency from top to bottom constitute axial hetero-junctions cylinder, institute
The surface of silicon oxide substrate and the surface setting transparent conductive film of the axial hetero-junctions cylinder are stated, the ZnO nano is located at
The surface setting metal grid lines electrode of the transparent conductive film of column periodic array structure two sides is as conductive electrode for dispatch from foreign news agency
Road driving.
Preferably, the silicon oxide substrate with a thickness of 20~2000 μm.
Preferably, the ZnO nano column diameter of the ZnO nano column periodic array structure is 100~800nm, is highly 100
~8000nm, duty ratio are 0.1~0.8.
Preferably, the perovskite nanometer column diameter of the perovskite nano-pillar periodic array structure is 100~800nm, high
Degree is 100~8000nm, and duty ratio is 0.1~0.8, and the perovskite is CH3NH3PbI3。
Preferably, the transparent conductive film is in molybdenum oxide, tin indium oxide, Al-Doped ZnO and Polyglycolic acid fibre
One kind, with a thickness of 200~800nm.
Preferably, the metal grid lines electrode is one of Au, Ag, Al, Gu and Pt, with a thickness of 20~1000nm.
A kind of preparation method of wide spectrum nano-array detector, comprising steps of being utilized on the surface of silicon oxide substrate
ZnO films grown by magnetron sputtering prepares perovskite thin film using spin-coating method on ZnO film surface, and it is enterprising then to place roasting glue machine
Row solid glue handles to obtain hetero-junctions substrate;The perovskite nanometer of consistency from top to bottom is prepared in the hetero-junctions substrate using laser ablation
Column periodic array and ZnO nano column periodic array, the perovskite nano-pillar and the ZnO nano column consistency from top to bottom constitute axial
Hetero-junctions cylinder;The hetero-junctions substrate after laser ablation is placed in vacuum chamber, is prepared using sputtering technology in the oxygen
The surface of silicon substrate and axial hetero-junctions damaged surface prepare transparent conductive film;Positioned at the ZnO nano column period battle array
The surface of the transparent conductive film of array structure two sides is using electron beam evaporation process preparation metal grid lines electrode as conduction
Electrode drives for external circuit.
Preferably, described that spin-coating method is utilized to drip perovskite solution described using sol evenning machine when preparing perovskite thin film
ZnO film surface, is placed on solid glue 30~200 minutes on roasting glue machine after even liquid, and 50~200 DEG C of solid glue temperature range.
The advantages of technical solution provided by the present invention, is: by ZnO nano column periodic array and perovskite nano-pillar week
The superposition of phase array constitutes axial hetero-junctions cylinder, has expanded the spectral response range of ZnO, has not lost ZnO ultraviolet spectra
The response of higher visible spectrum (450~800nm) is generated on the basis of (300~450nm) response, while excellent using ZnO
Carrier transport spy realize higher responsiveness.The present invention has the characteristics that simple structure, low cost and high-efficient, required work
Skill step is mature technology, is suitable for batch production.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of 1 wide spectrum nano-array detector of embodiment.
Fig. 2 is the spectral absorption of embodiment 1,2,3 wide spectrum nano-array detector and ZnO planar structure optical detector
Comparison diagram.
Fig. 3 is the electric-field intensity distribution figure of the 400nm photonic absorption of ZnO planar structure optical detector.
Fig. 4 is the electric-field intensity distribution figure of the 800nm photonic absorption of ZnO planar structure optical detector.
Fig. 5 is the electric-field intensity distribution figure of the 400nm photonic absorption of 1 wide spectrum nano-array detector of embodiment.
Fig. 6 is the electric-field intensity distribution figure of the 800nm photonic absorption of 1 wide spectrum nano-array detector of embodiment.
Fig. 7 is the electric-field intensity distribution figure of the 400nm photonic absorption of 2 wide spectrum nano-array detector of embodiment.
Fig. 8 is the electric-field intensity distribution figure of the 800nm photonic absorption of 2 wide spectrum nano-array detector of embodiment.
Fig. 9 is the electric-field intensity distribution figure of the 400nm photonic absorption of 3 wide spectrum nano-array detector of embodiment.
Figure 10 is the electric-field intensity distribution figure of the 800nm photonic absorption of 3 wide spectrum nano-array detector of embodiment.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but not as a limitation of the invention.
Incorporated by reference to shown in Fig. 1, the wide spectrum nano-array detector of embodiment 1 is made by following procedure: first in thickness
Degree is 50 μm, and the surface for the silicon oxide substrate 1 that purity is 99.996% utilizes ZnO films grown by magnetron sputtering, and target is using pure
The metal Zn target that degree is 99.99%, base vacuum are 2 × 10-4Pa, working gas are Ar and O2Mixed gas, operating air pressure
For 0.75Pa, 150 DEG C of silicon oxide substrate substrate temperature, the ZnO film with a thickness of 1000nm is prepared.It is utilized on ZnO film surface
Spin-coating method prepares perovskite thin film, by 0.318g (0.002mol) CH3NH3I (purity 99.5%) and 0.924g (0.002mol)
PbI2The small beaker that 1ml dinethylformamide solution is housed is added in (purity 99%).It is obtained after stirring
CH3NH3PbI3Perovskite solution is dripped on substrate using sol evenning machine, solid glue 100 on roasting glue machine is placed on after even liquid by spin coating liquid
Minute, 85 DEG C of solid glue temperature range, obtain the hetero-junctions substrate of the perovskite thin film with 1000nm thickness.Then laser is utilized
Etching technics completes nano column array preparation on hetero-junctions substrate, and laser uses wavelength 1064nm, the ND of pulsewidth 12ns:
YAG laser performs etching, and laser light incident angle is 0 degree, and pulsed irradiation number is 1.Axial hetero-junctions pillar array is 2 μm high, directly
Diameter 500nm, duty ratio 0.5.Then will there is the hetero-junctions substrate of axial hetero-junctions cylinder to be placed in vacuum chamber, utilizes sputtering work
The transparent conductive thin that a layer thickness is 200nm is deposited on the surface of silicon oxide substrate 1 and axial hetero-junctions damaged surface in skill
Film 4 utilizes electron beam evaporation process system in the two sides that 4 periphery of transparent conductive film is located at axial hetero-junctions cylinder periodic array
The metallic aluminium gate line electrode 5 of standby one layer of 20nm, two electrode extraction wires drive for external circuit and complete photocurrent detection.Wide spectrum
The specific structure of nano-array detector is silicon oxide substrate 1, and 2 periodic array of ZnO nano column is arranged in the surface of silicon oxide substrate 1
3 periodic array structure of perovskite nano-pillar, ZnO nano column 2 and calcium titanium is arranged in structure, 2 periodic array body structure surface of ZnO nano column
3 consistency from top to bottom of mine nano-pillar constitutes axial hetero-junctions cylinder, on the surface of silicon oxide substrate 1 and the surface of axial hetero-junctions cylinder
Transparent conductive film 4 is set, and the transparent conductive film 4 positioned at 2 periodic array structure two sides of ZnO nano column draws metallic aluminium grid line
Electrode 5 drives as conductive electrode for external circuit.
The wide spectrum nano-array detector of embodiment 2 is made by following procedure: first with a thickness of 50 μm, purity is
The surface of 99.996% silicon oxide substrate 1 utilize ZnO films grown by magnetron sputtering, target use purity for 99.99% gold
Belong to Zn target, base vacuum is 2 × 10-4Pa, working gas are Ar and O2Mixed gas, operating air pressure 0.75Pa, silica
150 DEG C of underlay substrate temperature, prepare the ZnO film with a thickness of 500nm.Perovskite is prepared using spin-coating method on ZnO film surface
Film, by 0.318g (0.002mol) CH3NH3I (purity 99.5%) and 0.924g (0.002mol) PbI2(purity 99%) adds
Enter the small beaker of 1ml dinethylformamide solution is housed.CH is obtained after stirring3NH3PbI3Spin coating liquid, utilizes sol evenning machine
By perovskite solution drop on substrate, it is placed on solid glue 100 minutes on roasting glue machine after even liquid, 85 DEG C of solid glue temperature range, obtains
The hetero-junctions substrate of perovskite thin film with 1500nm thickness.Then it is completed on hetero-junctions substrate using laser etching process
Nano column array preparation, laser use wavelength 1064nm, and the ND:YAG laser of pulsewidth 12ns performs etching, laser light incident angle
It is 0 degree, pulsed irradiation number is 1.Axial hetero-junctions pillar array is 2 μm high, diameter 500nm, duty ratio 0.5.Then will have
The hetero-junctions substrate of axial hetero-junctions cylinder is placed in vacuum chamber, surface and axis using sputtering technology in silicon oxide substrate 1
The transparent conductive film 4 that a layer thickness is 200nm is deposited to hetero-junctions damaged surface, ascends the throne on 4 periphery of transparent conductive film
The metallic aluminium gate line electrode of one layer of 50nm is prepared using electron beam evaporation process in the two sides of axial hetero-junctions cylinder periodic array
5, two electrode extraction wires drive for external circuit and complete photocurrent detection.
The wide spectrum nano-array detector of embodiment 3 is made by following procedure: first with a thickness of 50 μm, purity is
The surface of 99.996% silicon oxide substrate 1 utilize ZnO films grown by magnetron sputtering, target use purity for 99.99% gold
Belong to Zn target, base vacuum is 2 × 10-4Pa, working gas are Ar and O2Mixed gas, operating air pressure 0.75Pa, silica
150 DEG C of underlay substrate temperature, prepare the ZnO film with a thickness of 3000nm.Perovskite is prepared using spin-coating method on ZnO film surface
Film, by 0.318g (0.002mol) CH3NH3I (purity 99.5%) and 0.924g (0.002mol) PbI2(purity 99%) adds
Enter the small beaker of 1ml dinethylformamide solution is housed.CH is obtained after stirring3NH3PbI3Spin coating liquid, utilizes sol evenning machine
By perovskite solution drop on substrate, it is placed on solid glue 100 minutes on roasting glue machine after even liquid, 85 DEG C of solid glue temperature range, obtains
The hetero-junctions substrate of perovskite thin film with 3000nm thickness.Then it is completed on hetero-junctions substrate using laser etching process
Nano column array preparation, laser use wavelength 1064nm, and the ND:YAG laser of pulsewidth 12ns performs etching, laser light incident angle
It is 0 degree, pulsed irradiation number is 1.Axial hetero-junctions pillar array is 6 μm high, diameter 500nm, duty ratio 0.5.Then will have
The hetero-junctions substrate of axial hetero-junctions cylinder is placed in vacuum chamber, surface and axis using sputtering technology in silicon oxide substrate 1
The transparent conductive film 4 that a layer thickness is 200nm is deposited to hetero-junctions damaged surface, ascends the throne on 4 periphery of transparent conductive film
The metallic aluminium gate line electrode of one layer of 50nm is prepared using electron beam evaporation process in the two sides of axial hetero-junctions cylinder periodic array
5, two electrode extraction wires drive for external circuit and complete photocurrent detection.
The wide spectrum nano-array detector of embodiment 4 is made by following procedure: first with a thickness of 20 μm, purity is
The surface of 99.996% silicon oxide substrate 1 utilize ZnO films grown by magnetron sputtering, target use purity for 99.99% gold
Belong to Zn target, base vacuum is 2 × 10-4Pa, working gas are Ar and O2Mixed gas, operating air pressure 0.75Pa, silica
150 DEG C of underlay substrate temperature, prepare the ZnO film with a thickness of 100nm.Perovskite is prepared using spin-coating method on ZnO film surface
Film, by 0.318g (0.002mol) CH3NH3I (purity 99.5%) and 0.924g (0.002mol) PbI2(purity 99%) adds
Enter the small beaker of 1ml dinethylformamide solution is housed.CH is obtained after stirring3NH3PbI3Spin coating liquid, utilizes sol evenning machine
By perovskite solution drop on substrate, it is placed on solid glue 100 minutes on roasting glue machine after even liquid, 85 DEG C of solid glue temperature range, obtains
The hetero-junctions substrate of perovskite thin film with 100nm thickness.Then it is completed on hetero-junctions substrate using laser etching process
Nano column array preparation, laser use wavelength 1064nm, and the ND:YAG laser of pulsewidth 12ns performs etching, laser light incident angle
It is 0 degree, pulsed irradiation number is 1.Axial hetero-junctions pillar array is 0.2 μm high, diameter 100nm, duty ratio 0.1.It then will tool
There is the hetero-junctions substrate of axial hetero-junctions cylinder to be placed in vacuum chamber, using sputtering technology on the surface of silicon oxide substrate 1 and
The transparent conductive film 4 that a layer thickness is 400nm is deposited in axial hetero-junctions damaged surface, is on 4 periphery of transparent conductive film
The metallic aluminium grid line electricity of one layer of 400nm is prepared using electron beam evaporation process positioned at the two sides of axial hetero-junctions cylinder periodic array
Pole 5, two electrode extraction wires drive for external circuit and complete photocurrent detection.
The wide spectrum nano-array detector of embodiment 5 is made by following procedure: first with a thickness of 2000 μm, purity
Surface for 99.996% silicon oxide substrate 1 utilizes ZnO films grown by magnetron sputtering, and target uses purity for 99.99%
Metal Zn target, base vacuum are 2 × 10-4Pa, working gas are Ar and O2Mixed gas, operating air pressure 0.75Pa, oxidation
150 DEG C of silicon substrate substrate temperature, prepare the ZnO film with a thickness of 8000nm.Calcium titanium is prepared using spin-coating method on ZnO film surface
Mine film, by 0.318g (0.002mol) CH3NH3I (purity 99.5%) and 0.924g (0.002mol) PbI2(purity 99%)
The small beaker that 1ml dinethylformamide solution is housed is added.CH is obtained after stirring3NH3PbI3Spin coating liquid, utilizes spin coating
Machine drips perovskite solution on substrate, and solid glue 100 minutes on roasting glue machine are placed on after even liquid, 85 DEG C of solid glue temperature range, are obtained
To the hetero-junctions substrate of the perovskite thin film with 8000nm thickness.Then complete on hetero-junctions substrate using laser etching process
It is prepared at nano column array, laser uses wavelength 1064nm, and the ND:YAG laser of pulsewidth 12ns performs etching, laser light incident
Angle is 0 degree, and pulsed irradiation number is 1.Axial hetero-junctions pillar array is 16 μm high, diameter 800nm, duty ratio 0.8.It then will tool
There is the hetero-junctions substrate of axial hetero-junctions cylinder to be placed in vacuum chamber, using sputtering technology on the surface of silicon oxide substrate 1 and
The transparent conductive film 4 that a layer thickness is 600nm is deposited in axial hetero-junctions damaged surface, is on 4 periphery of transparent conductive film
The metallic aluminium grid line electricity of one layer of 500nm is prepared using electron beam evaporation process positioned at the two sides of axial hetero-junctions cylinder periodic array
Pole 5, two electrode extraction wires drive for external circuit and complete photocurrent detection.
It should be understood that each layer structural parameters are preferred parameter in the various embodiments described above, wherein the thickness of silicon oxide substrate 1 can
Think 20~2000 μm, transparent conductive film 4 is in molybdenum oxide, tin indium oxide, Al-Doped ZnO and Polyglycolic acid fibre
One kind, thickness can be 200~800nm, and metal grid lines electrode 5 is Au, Ag, Al, Gu or Pt, thickness can for 20~
1000nm, the solid glue time can be 30~200 minutes when preparing perovskite thin film, and 50~200 DEG C of solid glue temperature range.
Comparative example uses existing ZnO planar structure optical detector, figure it is seen that existing ZnO planar structure light is visited
It surveys wave-length coverage absorptivity of the device after 450nm to decline to a great extent, the embodiment 1,2,3 of perovskite-ZnO axial direction hetero-junctions is set
Compared with existing ZnO planar structure optical detector, the photonic absorbance of the visible wavelength in 450~800nm interval range is aobvious
It writes and improves, realize wide spectrum response.Electric-field intensity distribution figure from Fig. 3 to Figure 10 can be seen that embodiment 1,2,3 with it is existing
ZnO planar structure optical detector is compared, and 400nm photon and 800nm photon can be by axial perovskite nano-pillars and ZnO nano
Column absorbs respectively, and with the increase of nano-pillar height in array, the spectral responsivity of device also enhances therewith.
Claims (8)
1. a kind of wide spectrum nano-array detector, which is characterized in that including silicon oxide substrate, the surface of the silicon oxide substrate
ZnO nano column periodic array structure, the ZnO nano column periodic array body structure surface setting perovskite nano-pillar period battle array are set
Array structure, the ZnO nano column and the perovskite nano-pillar consistency from top to bottom constitute axial hetero-junctions cylinder, the silicon oxide liner
Transparent conductive film is arranged in the surface at bottom and the surface of the axial hetero-junctions cylinder, is located at the ZnO nano column periodic array
The surface setting metal grid lines electrode of the transparent conductive film of structure two sides drives as conductive electrode for external circuit.
2. wide spectrum nano-array detector according to claim 1, which is characterized in that the thickness of the silicon oxide substrate
It is 20~2000 μm.
3. wide spectrum nano-array detector according to claim 1, which is characterized in that the ZnO nano column period battle array
The ZnO nano column diameter of array structure is 100~800nm, is highly 100~8000nm, and duty ratio is 0.1~0.8.
4. wide spectrum nano-array detector according to claim 1, which is characterized in that the perovskite nano-pillar period
The perovskite nanometer column diameter of array structure is 100~800nm, is highly 100~8000nm, and duty ratio is 0.1~0.8, institute
Stating perovskite is CH3NH3PbI3。
5. wide spectrum nano-array detector according to claim 1, which is characterized in that the transparent conductive film is oxygen
Change one of molybdenum, tin indium oxide, Al-Doped ZnO and Polyglycolic acid fibre, with a thickness of 200~800nm.
6. wide spectrum nano-array detector according to claim 1, which is characterized in that the metal grid lines electrode is
One of Au, Ag, Al, Gu and Pt, with a thickness of 20~1000nm.
7. a kind of preparation method of wide spectrum nano-array detector as claimed in any of claims 1 to 6, special
Sign is, comprising steps of utilizing ZnO films grown by magnetron sputtering on the surface of silicon oxide substrate, utilizes on ZnO film surface
Spin-coating method prepares perovskite thin film, then places progress solid glue on roasting glue machine and handles to obtain hetero-junctions substrate;Using laser ablation
The perovskite nano-pillar periodic array and ZnO nano column periodic array of consistency from top to bottom, the calcium are prepared in the hetero-junctions substrate
Titanium ore nano-pillar and the ZnO nano column consistency from top to bottom constitute axial hetero-junctions cylinder;By the hetero-junctions after laser ablation
Substrate is placed in vacuum chamber, surface and axial hetero-junctions damaged surface using sputtering technology preparation in the silicon oxide substrate
Prepare transparent conductive film;Positioned at the surface benefit of the transparent conductive film of ZnO nano column periodic array structure two sides
Deposited by electron beam evaporation technique prepares metal grid lines electrode as conductive electrode and drives for external circuit.
8. the preparation method of wide spectrum nano-array detector according to claim 7, which is characterized in that described to utilize rotation
Perovskite solution is dripped in the silicon oxide substrate using sol evenning machine when coating prepares perovskite thin film, is placed on after even liquid roasting
Solid glue 30~200 minutes on glue machine, 50~200 DEG C of solid glue temperature range.
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Application publication date: 20190510 |