CN104819938A - Surface photovoltage measuring method with combination of modulated light and non-modulated light - Google Patents
Surface photovoltage measuring method with combination of modulated light and non-modulated light Download PDFInfo
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- CN104819938A CN104819938A CN201510262078.5A CN201510262078A CN104819938A CN 104819938 A CN104819938 A CN 104819938A CN 201510262078 A CN201510262078 A CN 201510262078A CN 104819938 A CN104819938 A CN 104819938A
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Abstract
The invention discloses a surface photovoltage measuring method with a combination of modulated light and non-modulated light and belongs to the technical field of semiconductor photovoltage measurement. The surface photovoltage measuring method comprises the following steps: putting a sample to be measured on an ITO conductive glass bottom electrode, covering the sample to be measured with a mica sheet with the thickness being 10-40 microns, and covering the mica sheet with an upper electrode; turning on a light source, enabling the modulated light and the non-modulated light to irradiate the sample to be measured simultaneously, amplifying a photovoltage signal generated between the bottom electrode and the upper electrode of the sample to be measured by a phase-locking amplifier, inputting the signal into a computer, recording the intensity value of the photovoltage signal of the sample to be measured by the computer, and further realizing the measurement for the surface photovoltage of the sample to be measured. The surface photovoltage measuring method disclosed by the invention has the advantages that by utilization of a detection result, the capturing action of a semiconductor surface state on photogenerated charge, the dynamic migration of bulk-phase photogenerated charge and the migration behavior of photogenerated charge of an all-solid-state Z-shaped semiconductor compound system can be directly discussed.
Description
Technical field
The invention belongs to technical field of new energy development, be specifically related to the measuring method of the novel photoelectric functional material surface photovoltage that a kind of light modulated combines with non-modulation light, exosyndrome material photogenerated charge transport property can be carried out by measured surface photovoltage.
Background technology
The research and preparation of novel photoelectric functional material plays vital effect to solution energy and environment problem, and in the research and development of novel optoelectronic materials, plays vital effect to the detection of the photoelectric properties of material.Surface photovoltaic spectroscopy is the very promising photoelectric properties detection means of one, there is the features such as highly sensitive, simple to operate, harmless sample, thus be widely used in the research of parsing photoelectric material photogenerated charge behavior (see Surface photovoltage phenomena:theory, experiment, andapplications, Surface Science Reports.1999,37,1-206).
Surface photovoltaic spectroscopy can be used for studying the photogenerated charge behavior of photogenerated charge under the surface effect of optical semiconductor sulfate ferroelectric functional material and interfacial effect affect.2004, the people such as Lin Yanhong demonstrate the existence of quantum dot ZnO photoelectric semiconductor material quantum confined effect (see A Study ofQuantum Confinement Properties of Photogenerated Charges in ZnONanoparticles by Surface Photovoltage Spectroscopy with surface photovoltaic spectroscopy, The Journal of PhysicalChemistry B.2004,108,3202-3206).2010, the people such as Dieter Gross successfully demonstrate the photogenerated charge transmission direction of Type II type semiconductor heterostructure (see ChargeSeparation in Type II Tunneling Multilayered Structures of CdTe and CdSeNanocrystals Directly Proven by Surface Photovoltage Spectroscopy with surface photovoltaic spectroscopy, Journalof the American Chemical Society.2010,132,5981 – 5983).
But, still there are many photoelectricities cannot to be proved by the surface photovoltage detection means reported.
Summary of the invention
The invention provides the surface photovoltage measuring method that a kind of light modulated combines with non-modulation light, the surface and interface information of the photoelectric semiconductor material that can more be enriched by the measurement of effects on surface photovoltage.
Conventional surface photovoltage measuring method as shown in Figure 1.As shown in Figure 2, its concrete steps are as follows for the photocoupler system surface photovoltage measuring method that a kind of light modulated of the present invention combines with non-modulation light:
(1) testing sample is placed on ITO electro-conductive glass hearth electrode, covers testing sample with 10 ~ 40 μm of thick mica sheets, then cover top electrode on mica sheet; In photovoltage sample cell, ITO electro-conductive glass hearth electrode connects ground connection by sample cell wire, and top electrode connects the signal input part connecing lock-in amplifier by sample cell wire, and the signal output part of lock-in amplifier connects computing machine;
(2) light source is opened, make light modulated and non-modulation light be irradiated to (conventional surface photovoltage does not use non-modulation illumination to penetrate in measuring) on testing sample simultaneously, testing sample due to photogenerated charge after illumination surface or Interface electric field effect under produce displacement, thus electric potential difference is produced between upper/lower electrode, (concrete principle is see Surface photovoltage phenomena:theory to be photoelectric signal, experiment, andapplications, Surface Science Reports.1999,37,1-206); The photoelectric signal produced between testing sample hearth electrode and top electrode is after lock-in amplifier amplifies, and input computing machine, by the photoelectric signal intensity level of computer recording testing sample, and then realizes the measurement to testing sample surface photovoltage.
Wherein, the wavelength 300 ~ 1000nm, the light intensity 0.1mW/cm that send of laser instrument or LED
2~ 100mW/cm
2monochromatic light as non-modulation light; Xenon lamp is that the light of 10 ~ 2000Hz is as light modulated by the frequency obtained after chopper by the monochromatic light of wavelength 1000 ~ 200nm of disperseing out after monochromator (scanning process should by long wave to shortwave scanning direction, corresponding by low photon energy to high photon energy scanning direction) again; Wherein, the wavelength of non-modulation light and concrete sweep limit (fixed wave length, the change frequency of light modulated during concrete measurement; Or fixed frequency, change wavelength) to determine according to the band gap of the amount for the treatment of sample, photon energy must produce photo-generate electron-hole pair by vitalizing semiconductor.
Wherein, testing sample can be that (organic semiconductor is as heteropoly acid, porphyrin, phthalocyanine, perylene class etc. for organic and inorganic semiconductor and organic/inorganic composite semiconductor photoelectric material; Inorganic semiconductor is as titania, zinc paste, cadmium sulfide, strontium titanates, di-iron trioxide etc.; Organic-inorganic composite semiconductor as titania cadmium sulfide composite material, titanium dioxide porphyrin compound substance), can be powder, monocrystalline or film; Top electrode is ITO or Pt wire netting.
Further, light modulated from power on pole irradiates the front of testing sample, and non-modulation light can irradiate the front of testing sample in pole from power on, also can irradiate the back side of testing sample from bottom electrode.
The present invention, compared with existing surface photovoltage measuring technique, can provide following effective information:
1) the present invention adopts photocoupler system to measure the photovoltage of photoelectric semiconductor material, when the non-modulation monochromatic light of specific wavelength (is selected based on sample band gap, photon energy must vitalizing semiconductor produce photo-generate electron-hole to) extremely incident from power on time, the surface state information of more abundant photoelectric semiconductor material can be provided, as by non-modulation monochromatic irradiation, make the surface state of photoelectric material by population, thus the photoelectric signal relevant to body phase photogenerated charge obtained under light modulated is irradiated, compared with the photoelectric signal relevant with surface state photogenerated charge under penetrating with the illumination of routine measurement system modulated, the corresponding relation in photogenerated charge and the body phase photogenerated charge life-span of being caught by surface state can be provided.
2) the present invention adopts photocoupler system to measure the photovoltage of photoelectric semiconductor material, when the non-modulation light of specific wavelength is incident from bottom electrode, can be used for proving all solid state Z-type interface photogenerated charge transfer process.
3) the present invention have simple to operate, provide the features such as photoelectric material surface and interface abundant information, be effectively supplementing of effects on surface photovoltage technique.
The present invention is on the basis that conventional surface photovoltage is tested, by the introducing of the non-modulation light with light modulated homonymy or heteropleural, effect can be caught by direct-detection semiconductor surface state to photogenerated charge, the Dynamic Migration process of body phase photogenerated charge, and the photogenerated charge migratory behaviour of all solid state Z-type interface semiconductors coupling system.The technological means that light modulated of the present invention combines with non-modulation light, by the introducing of simple non-modulation light, the important information of semiconductor material surface and interface photogenerated charge is provided, has expanded the intension of surface photovoltaic spectroscopy, enriched the detection system of surface photovoltaic spectroscopy.The means that the present invention adopts light modulated to combine with non-modulation light, have sample nondestructive, simple to operate, detect feature fast.
Accompanying drawing explanation
Fig. 1: conventional surface photovoltage measuring method schematic diagram;
Fig. 2: photocoupler system surface photovoltage measuring method schematic diagram;
Wherein, each several part name is called: xenon lamp 1, monochromator 2, chopper (modulating fan) 3, lens 4, catoptron 5, light modulated 6, lock-in amplifier 7, computing machine 8, non-modulation light 9.
Fig. 3: embodiment 1CdS nanowire surface photoelectricity press-fits quadrat method;
Each several part name is called: light modulated 6, non-modulation light 9, top electrode 10, bottom electrode 11, mica sheet 12, CdS nano wire 13;
Fig. 4: embodiment 1 conventional system CdS nanowire surface photovoltage spectrogram;
Fig. 5: embodiment 1 photocoupler system CdS nanowire surface photovoltage spectrogram;
Fig. 6: embodiment 1 conventional system CdS nano wire is based on the surface photovoltage spectrogram of modulating frequency;
Fig. 7: embodiment 1 photocoupler system CdS nano wire is based on the surface photovoltage spectrogram of modulating frequency;
Fig. 8: embodiment 2 photocoupler system TiO
2-Ti-ZnFe
2o
4ternary structural surface photovoltage measurement model (detects TiO
2side signal);
Each several part name is called: light modulated 6, non-modulation light 9, top electrode 10, bottom electrode 11, mica sheet 12, TiO
2layer 14, Ti layer 15, ZnFe
2o
4layer 16;
Fig. 9: embodiment 2 conventional system TiO
2side surface photovoltage spectrogram;
Figure 10: embodiment 2ZnFe
2o
4lower TiO is penetrated in the non-modulation illumination in side
2side surface photovoltage spectrogram;
Figure 11: embodiment 2 photocoupler system TiO
2-Ti-ZnFe
2o
4ternary structural surface photovoltage measurement model (detects ZnFe
2o
4side signal);
Each several part name is called: light modulated 6, non-modulation light 9, top electrode 10, bottom electrode 11, mica sheet 12, TiO
2layer 14, Ti layer 15, ZnFe
2o
4layer 16;
Figure 12: embodiment 2 conventional system ZnFe
2o
4side surface photovoltage spectrogram;
Figure 13: embodiment 2TiO
2lower ZnFe is penetrated in the non-modulation illumination in side
2o
4side surface photovoltage spectrogram.
Embodiment
Below by specific embodiment, the present invention is described, but is not limited thereto.
The embodiment of the present invention is raw materials used is commercially available analysis net product, without being further purified before using.
Embodiment 1
(1) measuring sample is that (synthetic method is see Solvothermal Synthesis of CdS Nanowires for Photocatalytic Hydrogen andElectricity Production for the cadmium sulfide nano wires of ethylenediamine water heat transfer, The Journal of Physical Chemistry C.2007,111,13280-13287).Measurement model is as shown in Figure 3: be placed in by cadmium sulfide nano wires on ITO hearth electrode, cover with 20 μm of mica sheets, then ITO top electrode is covered, put into photovoltage sample cell (all steel sample cell), top electrode connects lock-in amplifier input end by sample cell inside conductor, bottom electrode is by the external ground of sample cell inside conductor, and sample cell is full steel structure, can effectively shield ambient noise signal.
(2) do not apply non-modulation optical surface photovoltaic spectrum test result as shown in Figure 4, light modulated scanning wavelength is 800 ~ 300nm, and modulating frequency is 23Hz, and sample is irradiated in light modulated extreme direction from power on.There are two response districts in the CdS surface photovoltaic spectroscopy not applying non-modulation light, the surface state response district (it is donor surface state that negative signal illustrates) of 600 ~ 500nm respectively, and band band transition response district (now comprising a light induced electron too by surface state acquisition procedure) of 500 ~ 300nm.On this basis, the non-modulation light (5mW/cm of 532nm is applied
2laser pen, laserlands company), continue extreme direction from power on and irradiate sample, light modulated scanning wavelength is 800 ~ 300nm, under the photocoupler system obtained based on the surface photovoltaic spectroscopy measurement result of modulation wavelength as shown in Figure 5.Can observe, after applying non-modulation light, surface state response district disappears, band band transition response district signal strengthens, this is because the non-modulation light of 532nm continues to excite CdS valence-band electrons, makes the surface state of CdS keep population state, so this part the signal conductively-closed of surface state trapped electrons.In other words after being applied with non-modulation light, we can study separately the photogenerated charge behavior under the band band transition of CdS.
(3) under not applying non-modulation optical surface photovoltaic spectrum test condition, light modulated wavelength is fixed as 455nm, changes modulating frequency 11 ~ 1111Hz, obtain based on modulating frequency surface photovoltaic spectroscopy as shown in Figure 6.From step (2), now photoelectric signal is made up of two kinds of charge migration processes, and namely band band transition process and surface state catch light induced electron process.On this basis, the non-modulation light of 532nm continues extreme direction from power on and irradiates sample, and light modulated wavelength is fixed as 455nm, changes modulating frequency 10 ~ 1100Hz, obtains the photocoupler system surface photovoltaic spectroscopy based on modulating frequency, as shown in Figure 7.Now owing to the addition of the non-modulation light of 532nm, so signal is band band transition response separately.Contrast two figure known, in low frequency range, signal intensity difference is very large, and in high frequency region, signal intensity is more and more close.This illustrates that the photogenerated charge life-span that band band transition process produces is shorter, and the charge life of being caught by surface state is longer, so caught this part signal conductively-closed of electric charge in high frequency region by surface state, causes the signal intensity progressively unification of high frequency region.
From above result, the photovoltage scanning result carried out according to the method for embodiment 1 and general measuring method contrast mutually, effectively can provide the surface state information of sample, the surface state of CdS nano wire is donor surface state, and the photogenerated charge life-span will be longer than the body phase charge life-span.
Embodiment 2
(1) TiO
2-Ti-ZnFe
2o
4three-component compound system surface photovoltage is tested.Sample Preparation Procedure is: prepare two-sided TiO by electrochemistry anodic oxidation Ti paper tinsel
2nanotube, then a mirror polish exposes Ti substrate, continues with hanging painting method, load one deck ZnFe
2o
4(synthetic method is see Surface photovoltage phasespectra for analysing the photogenerated charge transfer and photocatalyticactivity of ZnFe
2o
4– TiO
2nanotube arrays, Physical Chemistry ChemicalPhysics.2013,15,14262-14269, unlike ZnFe
2o
4load is in the Ti substrate side of polishing).
(2) photocoupler system TiO
2-Ti-ZnFe
2o
4ternary structural TiO
2side surface photovoltage measurement model as shown in Figure 8, TiO
2-Ti-ZnFe
2o
4sample is placed on ITO hearth electrode, covers, then cover ITO top electrode with 20 μm of mica sheets, put into photovoltage sample cell, top electrode connects lock-in amplifier by sample cell inside conductor, and bottom electrode is by the external ground of sample cell inside conductor, sample cell is full steel structure, effectively shielding ambient noise signal.
(3), under not applying non-modulation optical surface photovoltaic spectrum test condition, light modulated irradiates sample TiO
2side, scanning wavelength is 500 ~ 300nm, and surface photovoltaic spectroscopy measurement result as shown in Figure 9.Non-modulation light (the 5mW/cm of 532nm
2laser pen, laserlands company) prolonged exposure sample ZnFe
2o
4side, sample TiO is irradiated in light modulated extreme direction from power on
2side, scanning wavelength is 500 ~ 300nm, and surface photovoltaic spectroscopy measurement result as shown in Figure 10.Two figure contrast known, ZnFe
2o
4when being continued to excite by the non-modulation light of 532nm with do not apply compared with non-modulation light, TiO
2side photoelectric signal strengthens to some extent, and TiO is described
2light induced electron in Ti substrate with ZnFe
2o
4photohole there occurs compound, make more photohole stay TiO
2side, so obtain stronger photoelectric signal.
(4) photocoupler system TiO
2-Ti-ZnFe
2o
4ternary structural ZnFe
2o
4side surface photovoltage measurement model as shown in figure 11, TiO
2-Ti-ZnFe
2o
4sample is placed on ITO hearth electrode, covers, then cover ITO top electrode with 20 μm of mica sheets, put into photovoltage sample cell, top electrode connects lock-in amplifier by sample cell inside conductor, and bottom electrode is by the external ground of sample cell inside conductor, sample cell is full steel structure, effectively shielding ambient noise signal.
(5), under not applying non-modulation optical surface photovoltaic spectrum test condition, light modulated irradiates sample ZnFe
2o
4side, scanning wavelength is 600 ~ 300nm, and surface photovoltaic spectroscopy measurement result as shown in figure 12.Non-modulation light (the 5mW/cm of 405nm
2laser pen, laserlands company) prolonged exposure sample TiO
2side, light modulated irradiates sample ZnFe
2o
4side, scanning wavelength is 600 ~ 300nm, and surface photovoltaic spectroscopy measurement result as shown in figure 13.Two figure contrast known, TiO
2when being continued to excite by the non-modulation light of 405nm with do not apply compared with non-modulation light, ZnFe2O4 side photoelectric signal weakens to some extent, within the scope of 600 ~ 420nm, even becomes a negative signal, ZnFe is described
2o
4photohole in Ti substrate with TiO
2light induced electron there occurs compound, make more light induced electron stay ZnFe
2o
4side, so obtain weak photovoltage positive signal, an even negative photoelectric signal.
From above result, the photovoltage scanning result carried out according to the method for embodiment 2 effectively can prove the process of Z-type semiconductor photoproduction transferring charge compared with general measuring method, semiconductor TiO
2and ZnFe
2o
4can there is recombination process in photogenerated charge, photogenerated charge is spatially separated in metal Ti.
Claims (6)
1. the surface photovoltage measuring method that combines with non-modulation light of light modulated, its step is as follows:
(1) testing sample is placed on ITO electro-conductive glass hearth electrode, covers testing sample with 10 ~ 40 μm of thick mica sheets, then cover top electrode on mica sheet; In photovoltage sample cell, ITO electro-conductive glass hearth electrode connects ground connection by sample cell wire, and top electrode connects the signal input part connecing lock-in amplifier by sample cell wire, and the signal output part of lock-in amplifier connects computing machine;
(2) light source is opened, light modulated and non-modulation light are irradiated on testing sample simultaneously, the photoelectric signal produced between testing sample hearth electrode and top electrode is after lock-in amplifier amplifies, input computing machine, by the photoelectric signal intensity level of computer recording testing sample, and then realize the measurement to testing sample surface photovoltage;
Wherein, the wavelength 300 ~ 1000nm, the light intensity 0.1mW/cm that send of laser instrument or LED
2~ 100mW/cm
2monochromatic light as non-modulation light; Xenon lamp is that the light of 10 ~ 2000Hz is as light modulated by the frequency obtained after chopper by the monochromatic light of wavelength 1000 ~ 200nm that disperses out after monochromator again; During concrete measurement, the wavelength of non-modulation light and the concrete sweep limit of light modulated are determined according to the band gap of the amount for the treatment of sample, and photon energy must produce photo-generate electron-hole pair by vitalizing semiconductor.
2. the surface photovoltage measuring method that combines with non-modulation light of a kind of light modulated as claimed in claim 1, is characterized in that: testing sample is organic and inorganic or organic-inorganic composite semiconductor photoelectric material.
3. the surface photovoltage measuring method that combines with non-modulation light of a kind of light modulated as claimed in claim 2, is characterized in that: photoconductive organic semiconductor material is heteropoly acid, porphyrin, phthalocyanine Huo perylene compounds; Inorganic semiconductor photoelectric material is titania, zinc paste, cadmium sulfide, strontium titanates or di-iron trioxide; Organic-inorganic composite semiconductor is titania cadmium sulfide composite material or titanium dioxide porphyrin compound substance.
4. the surface photovoltage measuring method that combines with non-modulation light of a kind of light modulated as claimed in claim 1, is characterized in that: testing sample is powder, monocrystalline or film.
5. the surface photovoltage measuring method that combines with non-modulation light of a kind of light modulated as claimed in claim 1, is characterized in that: top electrode is ITO or Pt wire netting.
6. the surface photovoltage measuring method that combines with non-modulation light of a kind of light modulated as claimed in claim 1, it is characterized in that: light modulated from power on pole irradiates the front of testing sample, non-modulation light from power on pole irradiates the front of testing sample or irradiates the back side of testing sample from hearth electrode.
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| CN107621567A (en) * | 2017-09-13 | 2018-01-23 | 吉林大学 | A kind of photoelectric semiconductor material transient photocurrents measuring system and measuring method |
| CN108051630A (en) * | 2017-12-08 | 2018-05-18 | 吉林大学 | A kind of method that photoelectric semiconductor material transient state photocurrent is measured under electric field or induced by magnetic field |
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| CN110470965B (en) * | 2019-07-09 | 2020-07-28 | 同济大学 | Semiconductor surface state carrier life test method |
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| CN110274900A (en) * | 2019-07-11 | 2019-09-24 | 长春工业大学 | A kind of monitoring method and system at original position real-time characterization inside solar energy battery interface |
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