CN111239098A - Method for detecting amorphous selenium charge neutral defect state - Google Patents

Method for detecting amorphous selenium charge neutral defect state Download PDF

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Publication number
CN111239098A
CN111239098A CN202010082045.3A CN202010082045A CN111239098A CN 111239098 A CN111239098 A CN 111239098A CN 202010082045 A CN202010082045 A CN 202010082045A CN 111239098 A CN111239098 A CN 111239098A
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amorphous selenium
pressure
defect state
raman
energy level
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杨凯锋
李恒梅
邹广田
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Jilin University
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Jilin University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering

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Abstract

The invention discloses a method for detecting amorphous selenium neutral defect state, belonging to the field of semiconductor material physical property detection, and comprising the following steps: step S1: putting an amorphous selenium sample into a diamond anvil cell pressing cavity, and applying pressure to the sample; step S2: measuring Raman scattering signals of amorphous selenium under different pressures; step S3: the defect state energy level is determined by analyzing the variation of the raman scattering intensity with pressure. The method provided by the invention is high in feasibility, simple and feasible, can effectively detect the electric neutral defect state of amorphous selenium caused by dihedral angle distortion, and can accurately determine the defect state energy level and the change relation of the defect state energy level with pressure.

Description

Method for detecting amorphous selenium charge neutral defect state
Technical Field
The invention belongs to the field of physical property detection of semiconductor materials, and particularly relates to a method for detecting an amorphous selenium neutral defect state.
Background
Amorphous selenium has attracted considerable attention from the past as a widely used semiconductor material, and studies on the properties of the semiconductor material have been conducted. The unique photosensitive property and the photoelectronic property of the amorphous selenium enable the amorphous selenium to have very important application value in a plurality of technical applications such as solar cells, photocopying technology, X-ray imaging, digital radiography and the like. Amorphous selenium exists in a plurality of defect state forms in a band gap, and is typically valence transformation pair coordination defects with negative correlation energy, intrinsic defects caused by dihedral distortion and the like, wherein the coordination defects form deep level defects with positive or negative charges according to the change of coordination numbers, and the dihedral distortion defects are shallow level defects with electric neutrality. The existence of the defect states has extremely important influence on the material characteristics of the amorphous selenium, and therefore, the accurate detection and characterization of the defect states of the amorphous selenium has extremely important significance on the popularization and application of the defect states and the development of new material characteristics.
At present, the more commonly used methods for detecting the defect state of a semiconductor include steady-state and transient photoconductive testing methods, photoinduced electron spin resonance and resonance raman scattering techniques, and the like. The steady-state and transient photoconductive test methods are successful in studying amorphous selenium defect state density, but the methods are generally more effective in detecting charged defect states because they rely on photoconductive property testing of the material, and the good insulating properties of the material due to the wide bandgap (1.95eV) of amorphous selenium at low temperatures do not facilitate accurate photoconductive testing; photoinduced electron spin resonance is only suitable for charged defect states and cannot be used for detecting neutral defect states, and the detection of electron spin resonance signals needs to be carried out in a low-temperature environment; although the resonance Raman scattering technology is an effective method for researching the transition between semiconductor bands, the detection of the amorphous selenium defect state by the technology is not realized at present. In summary, the detection of various defect states, particularly electrically neutral defect states, of amorphous selenium is still imperfect.
Disclosure of Invention
In view of the above, the present invention provides a method for detecting electrically neutral defect states of amorphous selenium by using a piezoresonance raman scattering technique, which is highly feasible, simple and feasible, and can effectively detect electrically neutral defect states of amorphous selenium caused by dihedral distortion.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for detecting the electric neutral defect state of amorphous selenium specifically comprises the following steps:
step S1: putting an amorphous selenium sample into a diamond anvil cell pressing cavity, and applying pressure to the sample;
step S2: measuring Raman scattering signals of amorphous selenium under different pressures;
step S3: the defect state energy level is determined by analyzing the variation of the raman scattering intensity with pressure.
Further, in step S1, the amorphous selenium sample is bulk amorphous selenium; in the diamond anvil cell, carrying out in-situ pressure calibration by using a ruby fluorescence method; t301 steel sheet 250 μm thick was used as a shim; a mixed solution of methanol, ethanol and water in a volume ratio of 16:3:1 is used as a pressure transmission medium.
Further, in step S2, a laser with a wavelength of 830nm in the near-infrared band is selected as an excitation light source; simultaneously detecting first-order and second-order Raman scattering peaks of the amorphous selenium chain molecular bond stretching vibration mode; and Raman scattering under different pressures is ensured to be carried out under the same test conditions of laser power, excitation area, focusing depth and the like.
Further, the step S3 specifically includes the following steps:
step S31: respectively obtaining the first-order and second-order Raman peak scattering intensity of the amorphous selenium chain molecular bond stretching vibration mode along with the pressure change, wherein the pressure range is from 0GPa to 4 GPa;
step S32: fitting Lorentz peak positions to the data in step S31 to determine the resonant pressure P of the corresponding first and second order Raman peaks1And P2；
Step S33: utilizing the linear change relation of defect state energy level with pressuren＝E0+(dE0/dP)PnObtaining defect state energy level E under zero voltage0And pressure coefficient dE thereof0(ii)/dP; where n has values of 1 and 2 corresponding to first and second order Raman peaks, EnFor the corresponding outgoing laser photon energy, i.e. the difference between the incident laser photon energy and the corresponding Raman vibration phonon energy, PnIs the resonance pressure P in the step S321And P2。
Compared with the prior art, the invention has the following advantages:
1. the method for detecting the amorphous selenium neutral defect state by utilizing the piezoresonance Raman scattering technology has high feasibility and is simple and easy to implement.
2. The method for detecting the electrically neutral defect state of the amorphous selenium by using the piezoresonance Raman scattering technology can effectively detect the electrically neutral defect state of the amorphous selenium caused by the dihedral angle distortion, and can accurately determine the defect state energy level and the change relation of the defect state energy level with the pressure.
Drawings
Figure 1 is a schematic view of a diamond anvil cell in an embodiment of the present invention.
Fig. 2 is a schematic diagram of a raman scattering test optical path used in an embodiment of the present invention.
Fig. 3 is raman scattering data of amorphous selenium at different pressures obtained in an example of the invention.
FIG. 4 is the amorphous selenium piezoresonance Raman peak scattering results obtained in the examples of the present invention.
Detailed Description
The technical scheme of the invention is specifically explained below with reference to the accompanying drawings. The invention relates to a method for detecting amorphous selenium electric neutral defect state by utilizing a piezoresonance Raman scattering technology. The energy level of the amorphous selenium in a charge neutral defect state caused by dihedral angle distortion and the change relation of the energy level with pressure can be obtained by accurately measuring the resonance pressure of first-order and second-order Raman peaks of a selenium amorphous selenium chain molecular bond stretching vibration mode, and the method specifically comprises the following steps:
step S1: putting an amorphous selenium sample into a diamond anvil cell pressing cavity, and applying pressure to the sample;
step S2: measuring Raman scattering signals of amorphous selenium under different pressures;
step S3: the defect state energy level is determined by analyzing the variation of the raman scattering intensity with pressure.
In the embodiment of the present invention, the assembly of the sample in the step S1 in the diamond anvil cell is as shown in fig. 1. In fig. 1, 11 is a pressure transmitting medium, 12 is an amorphous selenium sample, 13 is ruby particles, 14 is an upper pressure pad, 15 is an upper diamond anvil, 16 is a T301 steel shim, 17 is a lower diamond anvil, and 18 is a lower pressure pad. The conditions of step S1 are: the sample is amorphous selenium powder of bulk material; the diamond anvil has good light transmission and has no light absorption for light in the range from ultraviolet to infrared; carrying out in-situ pressure calibration by using a ruby fluorescence method; t301 steel sheet 250 μm thick was used as a shim; a mixed solution of methanol, ethanol and water with the volume ratio of 16:3:1 is used as a pressure transmission medium; the sample is pressurized by pressurizing the pallets up and down.
In this embodiment of the present invention, a schematic optical path diagram of the experimental system for raman scattering measurement in step S2 is shown in fig. 1. In fig. 2, 21 denotes a semiconductor laser, 22 denotes a laser, 23 denotes a laser beam expander, 24 denotes a sample, 25 denotes a microscope, 26 denotes a rayleigh filter set, 27 denotes a slit, 28 denotes a grating, and 29 denotes a ccd detector. The conditions of step S2 are: selecting 830nm wavelength laser of a near infrared band as an excitation light source; simultaneously detecting first-order and second-order Raman scattering peaks of the amorphous selenium chain molecular bond stretching vibration mode; and Raman scattering under different pressures is ensured to be carried out under the same test conditions of laser power, excitation area, focusing depth and the like.
Specifically, the raman scattering data at partial pressure obtained in the example of the present invention is shown in fig. 3. In FIG. 3, the solid line is the first order of the stretching vibrational mode of the amorphous selenium chain-like molecular bonds (with A) at pressures P of 0.16GPa and 0.91GPa1Expressed) and second order (with 2A)1Representation) raman peak, wherein the inset is an enlarged view of the second order raman peak.
In the embodiment of the present invention, the step S3 specifically includes the following steps:
step S31: the first-order and second-order Raman peak scattering intensity of the amorphous selenium chain molecular bond stretching vibration mode is obtained respectively along with the change of pressure, wherein the pressure range is from 0GPa to 4 GPa.
Step S32: fitting Lorentz peak positions to the data in step S31 to determine the resonant pressure P of the corresponding first and second order Raman peaks1And P2。
Step S33: utilizing the linear change relation of defect state energy level with pressuren＝E0+(dE0/dP)PnDetermination of the defect State energy level E at zero Voltage0And pressure thereofCoefficient of force dE0and/dP. Where n has values of 1 and 2 corresponding to first and second order Raman peaks, EnIs the corresponding outgoing laser photon energy (difference between the incident laser photon energy and the corresponding Raman vibration phonon energy), PnIs the resonance pressure P in the step S321And P2。
Specifically, FIG. 4 is a first order Raman peak (A) of bond stretching vibrational modes of amorphous selenium chain molecules according to an embodiment of the present invention1) And second order Raman peaks (2A)1) Pressure induced resonance raman results. In FIG. 4, the solid circle is A1The variation of Raman peak scattering intensity with pressure is 2A1The raman peak scattering intensity varies with pressure. The solid line is the corresponding Lorentzian peak position fitting result, P1And P2Is the resonance center pressure of the first and second order Raman peaks, respectively, obtained by fitting, where P1＝0.86GPa，P21.02 GPa. In addition, according to A in FIG. 31And 2A1The frequency shift position of Raman peak and the incident laser wavelength 830nm can be respectively used to obtain the energy E of emitted laser photon1＝1.467eV，E21.437 eV. Further, as described in step S33, the defect state energy level E corresponding to resonance Raman scattering at zero pressure can be solved01.64eV and the pressure coefficient dE of the defect state level0and/dP is-0.19 eV/GPa. Since the energy gap Eg of amorphous selenium is 1.95eV, the defect state is a shallow level defect with an energy of 0.31eV below the conduction band bottom, which is an electrically neutral defect state caused by dihedral distortion in the amorphous selenium chain molecule. In addition, the pressure coefficient (dE) of the defect state energy level obtained by the invention0-0.19eV/GPa vs. the pressure coefficient of the energy gap (dE)g-0.2eV/GPa) indicates that the defect state level varies almost in synchronism with the bandgap.
As can be seen from the above embodiments, the present invention provides a method for detecting electrically neutral defect states of amorphous selenium by using a piezoresonance Raman scattering technique, which has high feasibility and very high test accuracy, can effectively detect electrically neutral defect states of amorphous selenium caused by dihedral distortion, and can obtain the energy levels of the defect states and the change relationship thereof with pressure. The above embodiments are provided to explain the purpose, technical solutions and achievements of the present invention, and it should be understood that the above embodiments are only examples of the present invention, and not to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (4)

1. A method for detecting the electric neutral defect state of amorphous selenium specifically comprises the following steps:
step S1: putting an amorphous selenium sample into a diamond anvil cell pressing cavity, and applying pressure to the sample;
step S2: measuring Raman scattering signals of amorphous selenium under different pressures;
step S3: the defect state energy level is determined by analyzing the variation of the raman scattering intensity with pressure.
2. The method of claim 1, wherein in step S1, the amorphous selenium sample is bulk amorphous selenium; in the diamond anvil cell, carrying out in-situ pressure calibration by using a ruby fluorescence method; t301 steel sheet 250 μm thick was used as a shim; a mixed solution of methanol, ethanol and water in a volume ratio of 16:3:1 is used as a pressure transmission medium.
3. The method of claim 1, wherein in step S2, a laser with a wavelength of 830nm in the near infrared band is used as an excitation light source; simultaneously detecting first-order and second-order Raman scattering peaks of the amorphous selenium chain molecular bond stretching vibration mode; and Raman scattering under different pressures is ensured to be carried out under the same test conditions of laser power, excitation area, focusing depth and the like.
4. The method for detecting the electrically neutral defect state of amorphous selenium as claimed in claim 1, wherein said step S3 comprises the following steps:
step S31: respectively obtaining the first-order and second-order Raman peak scattering intensity of the amorphous selenium chain molecular bond stretching vibration mode along with the pressure change, wherein the pressure range is from 0GPa to 4 GPa;
step S32: fitting Lorentz peak positions to the data in step S31 to determine the resonant pressure P of the corresponding first and second order Raman peaks1And P2；
Step S33: utilizing the linear change relation of defect state energy level with pressuren＝E0+(dE0/dP)PnObtaining defect state energy level E under zero voltage0And pressure coefficient dE thereof0(ii)/dP; where n has values of 1 and 2 corresponding to first and second order Raman peaks, EnFor the corresponding outgoing laser photon energy, i.e. the difference between the incident laser photon energy and the corresponding Raman vibration phonon energy, PnIs the resonance pressure P in the step S321And P2。
CN202010082045.3A 2020-02-07 2020-02-07 Method for detecting amorphous selenium charge neutral defect state Pending CN111239098A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112945927A (en) * 2021-01-18 2021-06-11 吉林大学 In-situ high-pressure confocal Raman spectrum measurement system
CN114235822A (en) * 2021-12-28 2022-03-25 哈尔滨工业大学 Method for determining electron defect energy level of micro-area on processing surface of ultraviolet optical element

Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102507524A (en) * 2011-11-10 2012-06-20 大连理工大学 Method for diagnosing long-life electron metastable state of N2 in air plasma
CN109632861A (en) * 2019-01-29 2019-04-16 中国科学技术大学 A kind of high pressure magnetic resonance detection device

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102507524A (en) * 2011-11-10 2012-06-20 大连理工大学 Method for diagnosing long-life electron metastable state of N2 in air plasma
CN109632861A (en) * 2019-01-29 2019-04-16 中国科学技术大学 A kind of high pressure magnetic resonance detection device

Non-Patent Citations (1)

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Title
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112945927A (en) * 2021-01-18 2021-06-11 吉林大学 In-situ high-pressure confocal Raman spectrum measurement system
CN114235822A (en) * 2021-12-28 2022-03-25 哈尔滨工业大学 Method for determining electron defect energy level of micro-area on processing surface of ultraviolet optical element
CN114235822B (en) * 2021-12-28 2023-08-18 哈尔滨工业大学 Method for determining micro-area electronic defect energy level of ultraviolet optical element processing surface

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Application publication date: 20200605