CN106784318A - Methylamino halide CNT semiconductor light dependent sensor and preparation method - Google Patents
Methylamino halide CNT semiconductor light dependent sensor and preparation method Download PDFInfo
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- CN106784318A CN106784318A CN201611078395.2A CN201611078395A CN106784318A CN 106784318 A CN106784318 A CN 106784318A CN 201611078395 A CN201611078395 A CN 201611078395A CN 106784318 A CN106784318 A CN 106784318A
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- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/60—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation in which radiation controls flow of current through the devices, e.g. photoresistors
- H10K30/65—Light-sensitive field-effect devices, e.g. phototransistors
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- H—ELECTRICITY
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Abstract
The present invention relates to methylamino halide CNT semiconductor light dependent sensor and preparation method, light sensor includes the silicon chip of cleaning, drying as substrate；Hot pressing CNT regulates and controls layer as grid voltage on silicon chip；Spin coating methylamino halide is used as light absorbing zone on grid voltage regulation and control layer；Gold thin film is deposited with the top of light absorbing zone, after being blocked using mask plate as source electrode and drain electrode.Compared with prior art, methylamino halide and CNT physical bond are formed composite semiconductor by the present invention, by regulating and controlling the effect that grid voltage makes it possess Current amplifier, and can increase its photosensitive response degree.
Description
Technical field
The present invention relates to light sensor technical field, partly led more particularly, to a kind of methylamino halide-CNT
Body light sensor and preparation method.
Background technology
Light sensor be using semiconductor photoelectric effect, convert optical signal into a class photovoltaic device of electric signal output
Part.The every field of its and national economy military in remote sensing, night vision, investigation, imaging etc. is all widely used.In recent years to light
Lie prostrate in the research of device, the perovskite-type material of hybrid inorganic-organic is due to superior absorbing properties, regulatable band
Gap width, excellent carrier transmission performance and simple economic preparation method are widely used in solar cell.Wherein with
Nowadays perovskite-type material has been over 22% as the efficiency of the solar cell of light absorbing zone.Perovskite-type material is in light
Also it is extensively studied and application in dependent sensor field.Perovskite light sensor in addition to above-described advantage, this
The inferior position that body is present is that photoelectric current is small, does not possess grid voltage ability of regulation and control, and its photosensitive response degree is very small.Therefore will
It is it is obtained one of grid voltage regulating effect, the approach for improving photosensitive response degree that it is combined with other semi-conducting materials.
CNT is made up of cylindrical type graphite linings, with superior electric property and mechanical performance.Its diameter
Distribution is small, defect is few, with uniformity consistency higher.According to research reports, there is CNT root grid voltage to adjust
The function that control electric current, signal amplify, is one of the material for preparing inorganic field effect transistor.But its defect for existing is to visible
Light is not responding to.
Chinese patent CN105116033A discloses a kind of photosensitive copolymers composite carbon nanometer tube molecular engram sensor
Preparation method, obtains the compound self-assembly of molecular engram, then with the compounding assembling of photosensitive copolymers, CNT and template molecule
To modified electrode surface, eluted template molecule is that can obtain molecular imprinting electrochemical sensor to drop coating after photocrosslinking, its
Invention preparation process is carried out in water phase completely, with it is environment-friendly the characteristics of.CNT in the patent is received for many wall carbon
Mitron, shows as metallicity, and its photosensitive copolymers composite carbon nanometer tube is prepared using blending, and the single in this patent
It is semiconductive to manage, and is prepared using layering.
The content of the invention
The purpose of the present invention be exactly provide one kind for the defect for overcoming above-mentioned prior art to exist can be by regulating and controlling grid
Pressure makes it possess the effect of Current amplifier, and increases the methylamino halide-CNT semiconductor photosensitive of its photosensitive response degree
Sensor and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：
Methylamino halide-CNT semiconductor light dependent sensor, including：
The silicon chip of cleaning, drying is used as substrate；
Hot pressing CNT regulates and controls layer as grid voltage on silicon chip；
Spin coating methylamino halide is used as light absorbing zone on grid voltage regulation and control layer；
Gold thin film is deposited with the top of light absorbing zone, after being blocked using mask plate as source electrode and drain electrode.
The upper surface of described silicon chip also length has the about silicon dioxide insulating layer of 300nm.
Described CNT is SWCN, and its a diameter of 10-20nm, length is about 1-5 μm, and unit area is dense
Degree is located at 100-500ng/cm2。
Described grid voltage regulation and control layer is carbon nanotube layer, photosensitive with methylamino halide positioned at silicon dioxide insulating layer
Between layer.
Described methylamino halide can be CH3NH3PbI3、CH3NH3PbBr3、CH3NH3PbIxCl3-xDeng.
Described light absorbing zone is methylamino halide layer, and its thickness is about 300-500nm.
The preparation method of methylamino halide-CNT semiconductor light dependent sensor, using following steps：
(1) will be cleaned by ultrasonic through acetone, isopropanol as the silicon chip of substrate, after being rinsed with deionized water and alcohol,
Nitrogen dries up its surface；
(2) CNT is scattered in surfactant solution, carries out suction filtration, hot pressing film forming is carried out afterwards；
(3) methylamino halide precursor solution is spun on CNT；
(4) sample after spin coating is placed on warm table and anneals；
(5) sample is carried out into gold evaporation as electrode under the blocking of mask plate, that is, makes and obtain light sensor.
Surfactant solution described in step (2) uses neopelex solution, and CNT is molten
Solution is scattered in the concentration about 0.1-0.5mg/mL in above-described surfactant.Temperature is during CNT hot pressing film forming
100 DEG C, time 1h, hot pressing pressure is about 0.4-0.8MPa.
Spin coating rotating speed described in step (3) is 1000-4000rpm, and the time is 30s.
Methylamino halide precursor liquid solution can be prepared according to following steps：
Step one：It is pure that the chemical reagent purity bought is analysis.By the methylamine solution that 15ml mass fractions are 33%
It is added in the round-bottomed flask of 50ml, is added dropwise over the hydroiodic acid that 14ml mass fractions are 55%.The mixed solution is placed in ice bath
After middle reaction 2 hours, unnecessary solvent is evaporated dry with Rotary Evaporators.The crude product for obtaining will be rotated and be transferred to Buchner funnel
In, cleaned with absolute ether and acetonitrile solution at least three times, remove elemental iodine that may be present.The white that filtering and washing is obtained is consolidated
Body is put in and dried overnight in 55 DEG C of vacuum drying chamber standby obtains pure methylamino iodate amine (CH3NH3I), institute in experiment
The methylamino ammonium chloride for needing also according to said method is prepared.
Step 2：It is pure that the chemical reagent purity bought is analysis.Weigh lead iodide 0.46g (1mmol), methylamino iodine
Change amine 0.16g (1mmol), methylamino ammonium chloride 0.07g (1mmol) adds DMF (DMF) the stirring 1h of 1ml
Above until solid all dissolving, solution clarifications, filtered with the filtering head that aperture is 0.45 μm and obtain CH3NH3PbI3Forerunner
Liquid solution.
Sample is placed in the 0.5h that annealed on 100 DEG C of warm table by step in (4).
Compared with prior art, the present invention has advantages below：
1st, the composite semiconductor light sensor for preparing, has grid voltage regulating effect and light sensitive effect concurrently.Methylamino lead iodide
Good level-density parameter is formed with CNT, photo-generated carrier is efficiently separated at both interfaces, hole transition to carbon nanometer
Tube layer is simultaneously collected by gold electrode.Finally the photoelectric current of composite semiconductor light sensor is set to have reached microampere rank, and its is photosensitive
Responsiveness has reached 103。
2nd, the composite semiconductor light sensor for preparing, has grid voltage regulating effect and light sensitive effect concurrently.Add by grid
Voltage triggers electric current in carbon nano tube surface, and the big of carbon nano tube surface electric current is controlled by the intensity of control gate voltage
It is small.Equally there is semiconductor light dependent sensor after compound grid voltage to regulate and control the effect of electric current.
3rd, preparation process is simple, it is with low cost.
Brief description of the drawings
Fig. 1 is the main structure diagram of light sensor；
Fig. 2 is the overlooking the structure diagram of light sensor；
Fig. 3 is light sensor in illumination 4.5mW/cm2Photoelectric current and the photosensitive biography of methylamino halide under illumination condition
The photoelectric current contrast of sensor.
Fig. 4 closes the transfer curve changed with intensity of illumination for the brightness current switch of light sensor.
Fig. 5 is right with the photosensitive response degree of methylamino halide light sensor for the photosensitive response degree of light sensor
Than.
In figure, 1- substrates, 2- grid voltages regulation and control layer, 3- light absorbing zones, 4- gold thin films.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
Methylamino halide-CNT semiconductor light dependent sensor, its structure as shown in Figure 1-2, including cleaning, drying
Silicon chip as substrate 1, in the upper surface of silicon chip, also length has silica, and hot pressing CNT is used as grid voltage on silicon chip
Regulation and control layer 2；Spin coating methylamino halide is used as light absorbing zone 3 on grid voltage regulation and control layer；At the top of light absorbing zone, using covering
Film version is deposited with gold thin film 4 as source electrode and drain electrode after blocking.
Made using following methods and obtained：
The first step：During silicon chip is sequentially placed into acetone, aqueous isopropanol after each ultrasonic cleaning, rushed with deionized water, ethanol
After washing, dried up with nitrogen, be placed in dry for standby in baking oven.
Second step：CNT is scattered in surfactant solution, suction filtration is carried out, hot pressing film forming is carried out afterwards；
3rd step：Methylamino halide precursor liquid solution is spun on the CNT prepared in second step, is placed in
Anneal 0.5h on 100 DEG C of warm tables, obtains methylamino halide and CNT composite semiconductor filmses.
4th step：Evaporation thickness in vacuum evaporation instrument is placed in after composite semiconductor is blocked with the mask plate specified to be about
The gold electrode of 50nm.
Wherein, the methylamino halide precursor liquid solution that the 3rd step is used can be prepared according to following steps：
Step one：It is pure that the chemical reagent purity bought is analysis.By the methylamine solution that 15ml mass fractions are 33%
It is added in the round-bottomed flask of 50ml, is added dropwise over the hydroiodic acid that 14ml mass fractions are 55%.The mixed solution is placed in ice bath
After middle reaction 2 hours, unnecessary solvent is evaporated dry with Rotary Evaporators.The crude product for obtaining will be rotated and be transferred to Buchner funnel
In, cleaned with absolute ether and acetonitrile solution at least three times, remove elemental iodine that may be present.The white that filtering and washing is obtained is consolidated
Body is put in and dried overnight in 55 DEG C of vacuum drying chamber standby obtains pure methylamino iodate amine (CH3NH3I), institute in experiment
The methylamino ammonium chloride for needing also according to said method is prepared.
Step 2：It is pure that the chemical reagent purity bought is analysis.Weigh lead iodide 0.46g (1mmol), methylamino iodine
Change amine 0.16g (1mmol), methylamino ammonium chloride 0.07g (1mmol) adds DMF (DMF) the stirring 1h of 1ml
Above until solid all dissolving, solution clarifications, filtered with the filtering head that aperture is 0.45 μm and obtain CH3NH3PbI3Forerunner
Liquid solution.
The methylamino halide for preparing-CNT semiconductor light dependent sensor can carry out table using following methods
Levy：
A) light sensor is positioned on the probe station of semiconductor system Keithley 4200, opens light source, carry out crystalline substance
Body pipe transfer curve is tested, and the transfer curve of methylamino halide and CNT composite semiconductor shows, the film after being combined
With grid voltage regulating and controlling effect, and transistor after integrating is presented P-type semiconductor effect, brilliant when grid voltage is negative pressure and when increasing
The source-drain current increase of body pipe；And as intensity of illumination increases, the source-drain current (photoelectric current) of transistor further increases.
B) light sensor is positioned on the probe station of semiconductor system Keithley 4200, opens light source, carry out crystalline substance
Body pipe curve of output is tested, and sets different grid voltages, and knowable to the curve of output, grid negative pressure is bigger, the source of transistor
Leakage current is bigger；And as intensity of illumination increases, source-drain current (photoelectric current) the also further increase of transistor；And the source for measuring
There is good linear relationship in leakage current, it was demonstrated that there is good ohm between composite semiconductor and metal electrode with intensity of illumination
Contact.
Embodiment 2
The methylamino halide and the light sensor of CNT composite semiconductor prepared to embodiment 1 carry out electrical property
Can test, its transfer curve is tested with semiconductor test system, draw the change as grid voltage changes of its source-drain current
Curve, and in 4.5mW/cm2Illumination under transfer curve.Three curves are respectively methylamino halide, compound half in Fig. 3
Conductor light sensor is in the photocurrent curve for being not added with grid voltage and under the conditions of grid voltage is -60V.Can be obtained by curve in Fig. 3, this technology
The photoelectric current of the composite semiconductor light sensor of preparation is greatly improved compared with the photoelectric current of pure methylamino halide.It is being not added with
During grid voltage, under conditions of source-drain voltage is -20V, photoelectric current reaches 50 μ A, when grid voltage is -60V, the light under the same terms
Electric current has exceeded 100 μ A.Test result shows that the composite semiconductor light sensor of present invention preparation has in terms of photoelectric current
The breakthrough of the order of magnitude, and fully possess grid voltage regulation and control electric current, the function of signal amplification.
Embodiment 3
The methylamino halide and the light sensor and pure methylamino of CNT composite semiconductor prepared to embodiment 1
Halide light sensor carries out further optical performance test, and it is tested in different illumination bars with semiconductor test system
The transfer current of part.The curve that Fig. 4 changes for the brightness current on/off ratio of composite semiconductor light sensor with intensity of illumination.By
Figure understands that brightness current on/off ratio increases with the increase of intensity of illumination, and increases with the increase of grid negative pressure.Work as light
It is 40mW/cm according to intensity2When, under conditions of source-drain voltage is -20V, the on-off ratio of its grid voltage is 1.25.Test result
Show that the composite semiconductor light sensor of present invention preparation has grid voltage regulating effect and light sensitive effect concurrently.
Embodiment 4
The photosensitive response degree (Responsivity) of composite semiconductor light sensor is calculated, its computing formula is：
Wherein, ILightIt is photoelectric current, IDarkIt is dark current, PLightIt is incident intensity, A is effective irradiated area.Can by Fig. 5
, the photosensitive response degree of device reduces as intensity of illumination increases, with being consistent for being reported in document.When grid voltage is 0,
The photosensitive response degree of device contrasts the photosensitive response degree (less than 1A/W) of methylamino halide more than 1000A/W, improves 3
The order of magnitude；When grid voltage is -40V, the photosensitive response degree of device contrasts the photosensitive of methylamino halide more than 5000A/W
Responsiveness, improves 4 orders of magnitude.It is superior that test result proves that composite semiconductor light sensor prepared by the present invention has
Photo absorption property, and grid voltage regulation and control, the function that signal amplifies is clearly.
Embodiment 5
Methylamino halide-CNT semiconductor light dependent sensor, including cleaning, drying silicon chip as substrate, in silicon
Hot pressing CNT as grid voltage regulation and control layer, on grid voltage regulation and control layer, as light inhale by spin coating methylamino halide on piece
Receive layer, be deposited with gold thin film as source electrode and drain electrode at the top of light absorbing zone, after being blocked using mask plate.
Wherein, the upper surface of silicon chip also length has the about silicon dioxide insulating layer of 300nm, and the CNT for using is single wall
CNT, its a diameter of 10nm, length is about 1 μm, and per unit area concentration is located at 100ng/cm2.Light absorbing zone is methylamino
Halide layer, methylamino halide is CH3NH3PbBr3, its thickness is 300nm.
The preparation method of methylamino halide-CNT semiconductor light dependent sensor, using following steps：
(1) will be cleaned by ultrasonic through acetone, isopropanol as the silicon chip of substrate, after being rinsed with deionized water and alcohol,
Nitrogen dries up its surface；
(2) CNT is scattered in neopelex solution, CNT concentration in the solution is
0.1mg/mL, then carries out suction filtration, and hot pressing film forming is carried out afterwards, and temperature is 100 DEG C, time 1h, hot pressing pressure during hot pressing film forming
It is 0.4MPa；
(3) by methylamino halide CH3NH3PbBr3Precursor solution be spun on CNT, spin coating rotating speed is
1000rpm, the time is 30s；
(4) sample after spin coating is placed in the 0.5h that annealed on 100 DEG C of warm table；
(5) sample is carried out into gold evaporation as electrode under the blocking of mask plate, that is, makes and obtain light sensor.
Embodiment 6
Methylamino halide-CNT semiconductor light dependent sensor, including cleaning, drying silicon chip as substrate, in silicon
Hot pressing CNT as grid voltage regulation and control layer, on grid voltage regulation and control layer, as light inhale by spin coating methylamino halide on piece
Receive layer, be deposited with gold thin film as source electrode and drain electrode at the top of light absorbing zone, after being blocked using mask plate.
Wherein, the upper surface of silicon chip also length has the about silicon dioxide insulating layer of 350nm, and the CNT for using is single wall
CNT, its a diameter of 20nm, length is about 5 μm, and per unit area concentration is located at 500ng/cm2.Light absorbing zone is methylamino
Halide layer, methylamino halide is CH3NH3PbIxCl3-x, x can be 0-3, and its thickness is 500nm.
The preparation method of methylamino halide-CNT semiconductor light dependent sensor, using following steps：
(1) will be cleaned by ultrasonic through acetone, isopropanol as the silicon chip of substrate, after being rinsed with deionized water and alcohol,
Nitrogen dries up its surface；
(2) CNT is scattered in neopelex solution, CNT concentration in the solution is
0.5mg/mL, then carries out suction filtration, and hot pressing film forming is carried out afterwards, and temperature is 100 DEG C, time 1h, hot pressing pressure during hot pressing film forming
It is 0.8MPa；
(3) by methylamino halide CH3NH3PbIxCl3-xPrecursor solution be spun on CNT, spin coating rotating speed is
4000rpm, the time is 30s；
(4) sample after spin coating is placed in the 0.5h that annealed on 100 DEG C of warm table；
(5) sample is carried out into gold evaporation as electrode under the blocking of mask plate, that is, makes and obtain light sensor.
Claims (10)
1. methylamino halide-CNT semiconductor light dependent sensor, it is characterised in that the light sensor includes：
The silicon chip of cleaning, drying is used as substrate；
Hot pressing CNT regulates and controls layer as grid voltage on silicon chip；
Spin coating methylamino halide is used as light absorbing zone on grid voltage regulation and control layer；
Gold thin film is deposited with the top of light absorbing zone, after being blocked using mask plate as source electrode and drain electrode.
2. methylamino halide according to claim 1-CNT semiconductor light dependent sensor, it is characterised in that institute
The upper surface of the silicon chip stated also length has the silicon dioxide insulating layer that thickness is 280-350nm.
3. methylamino halide according to claim 1-CNT semiconductor light dependent sensor, it is characterised in that institute
The CNT stated is SWCN, and its a diameter of 10-20nm, length is 1-5 μm, and per unit area concentration is located at 100-
500ng/cm2。
4. methylamino halide according to claim 2-CNT semiconductor light dependent sensor, it is characterised in that institute
The grid voltage regulation and control layer stated is carbon nanotube layer, between silicon dioxide insulating layer and methylamino halide photosensitive layer.
5. methylamino halide according to claim 1-CNT semiconductor light dependent sensor, it is characterised in that institute
The methylamino halide stated is CH3NH3PbI3、CH3NH3PbBr3Or CH3NH3PbIxCl3-x。
6. methylamino halide according to claim 1-CNT semiconductor light dependent sensor, it is characterised in that institute
The light absorbing zone stated is methylamino halide layer, and its thickness is 300-500nm.
7. as disclosed in any one of claim 1-6 methylamino halide-CNT semiconductor light dependent sensor preparation
Method, it is characterised in that the method uses following steps：
(1) will be cleaned by ultrasonic through acetone, isopropanol as the silicon chip of substrate, after being rinsed with deionized water and alcohol, nitrogen
Dry up its surface；
(2) CNT is scattered in surfactant solution, carries out suction filtration, hot pressing film forming is carried out afterwards；
(3) methylamino halide precursor solution is spun on CNT；
(4) sample after spin coating is placed on warm table and anneals；
(5) sample is carried out into gold evaporation as electrode under the blocking of mask plate, that is, makes and obtain light sensor.
8. the preparation method of methylamino halide according to claim 7-CNT semiconductor light dependent sensor, it is special
Levy and be, the surfactant solution described in step (2) is neopelex solution, CNT dissolving is scattered in
In above-described surfactant solution, concentration is 0.1-0.5mg/mL.Temperature is 100 DEG C during CNT hot pressing film forming,
Time 1h, hot pressing pressure is 0.4-0.8MPa.
9. the preparation method of methylamino halide according to claim 7-CNT semiconductor light dependent sensor, it is special
Levy and be, the spin coating rotating speed described in step (3) is 1000-4000rpm, and the time is 30s.
10. the preparation method of methylamino halide according to claim 7-CNT semiconductor light dependent sensor, its
It is characterised by, sample is placed in the 0.5h that annealed on 100 DEG C of warm table by step in (4).
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| US20210241979A1 (en) * | 2020-01-14 | 2021-08-05 | Tianjin University | Wide spectrum detector and preparation method |
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Application publication date: 20170531 |