CN113937023A - Method for testing defect influence energy transfer in two-dimensional material heterojunction - Google Patents
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- 238000012546 transfer Methods 0.000 title claims abstract description 73
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- 238000011282 treatment Methods 0.000 claims abstract description 12
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical group S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 39
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 38
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical group S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims description 35
- 229910052582 BN Inorganic materials 0.000 claims description 32
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 32
- 238000012545 processing Methods 0.000 claims description 25
- 238000003384 imaging method Methods 0.000 claims description 16
- 230000001052 transient effect Effects 0.000 claims description 8
- 238000001237 Raman spectrum Methods 0.000 claims description 7
- 238000000103 photoluminescence spectrum Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000001506 fluorescence spectroscopy Methods 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
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Abstract
The invention provides a method for testing the influence of defects in a two-dimensional material heterojunction on energy transfer, which relates to the technical field of semiconductors and comprises the following steps: placing a single-layer lower-layer transition metal sulfide, an isolation layer and a single-layer upper-layer transition metal sulfide in sequence from bottom to top to prepare a heterojunction; performing plasma treatment on the heterojunction for several times to introduce defects into the heterojunction, wherein the first treatment time is equal to 0 second; and detecting the heterojunction after the heterojunction is subjected to plasma treatment every time. The isolation layer is arranged, so that a gap is formed between the lower transition metal sulfide and the upper transition metal sulfide, and the influence of charge transfer between the lower transition metal sulfide and the upper transition metal sulfide on the accuracy of a test result is avoided. The influence of the defects on the energy transfer of the heterojunction can be obtained by detecting the energy transfer conditions of the heterojunction after plasma treatment at different time.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a method for testing influence of defects in a two-dimensional material heterojunction on energy transfer.
Background
Energy transfer is a non-radiative transfer process from a donor to an acceptor, and has led to extensive research in various photovoltaic applications including solar cells, light emitting diodes, and lasers due to its high energy conversion efficiency and strong emission characteristics.
In nanoscale semiconductor hybrid structures, energy transfer between different materials is often the cause of their photoresponse. Since transition metal sulfides (TMDC) have a strong exciton effect, different two-dimensional TMDCs can be coupled by van der waals force to form a heterojunction, which is used to study energy transfer between different materials.
However, due to the low coulomb shielding effect and the high sensitivity to intrinsic doping, defects are easily introduced in TMDC during production or operation, thereby strongly influencing the electronic structure and optical bandgap of TMDC, and ultimately the energy transfer between materials. Understanding the effect of defects on the energy transfer kinetics of two-dimensional TMDC heterostructures is very important for the development of TMDC heterostructure-based optoelectronic devices.
Therefore, the invention aims to provide a method for testing defects in a two-dimensional material heterojunction to influence energy transfer.
Disclosure of Invention
The invention aims to provide a method for testing defects in a two-dimensional material heterojunction to influence energy transfer.
The invention provides a method for testing the influence of defects in a two-dimensional material heterojunction on energy transfer, which comprises the following steps:
placing a single-layer lower-layer transition metal sulfide, an isolation layer and a single-layer upper-layer transition metal sulfide in sequence from bottom to top to prepare a heterojunction;
carrying out plasma treatment on the heterojunction for several times to introduce defects into the heterojunction, wherein the first treatment time is 0 second;
and detecting the heterojunction after the heterojunction is subjected to plasma treatment every time.
According to the method for testing the defect influence energy transfer in the two-dimensional material heterojunction, the detection of the heterojunction comprises the following steps:
detecting the heterojunction by a steady state fluorescence spectroscopy technique to obtain a PL spectrum of the heterojunction for a corresponding processing time; and/or the presence of a gas in the gas,
and detecting the heterojunction by a transient fluorescence lifetime imaging technology to obtain a fluorescence lifetime imaging graph and a fluorescence lifetime attenuation curve of the heterojunction at corresponding processing time.
According to the method for testing the defect influence energy transfer in the two-dimensional material heterojunction, after the obtaining of the fluorescence lifetime decay curve of the heterojunction at the corresponding processing time, the method further comprises the following steps:
fitting the fluorescence lifetime decay curve to obtain exciton lifetime and average exciton lifetime;
calculating an energy transfer rate and an energy transfer efficiency from the average exciton lifetime.
According to the method for testing the defect influence energy transfer in the two-dimensional material heterojunction, before the several times of plasma treatment on the heterojunction, the method further comprises the following steps:
and respectively verifying the lower-layer transition metal sulfide and the upper-layer transition metal sulfide through a steady-state Raman spectrum characteristic peak value and a characteristic peak value difference.
According to the method for testing the defect influence energy transfer in the two-dimensional material heterojunction, before the several times of plasma treatment on the heterojunction, the method further comprises the following steps:
and respectively detecting the thicknesses of the lower-layer transition metal sulfide, the upper-layer transition metal sulfide and the isolation layer of the heterojunction to determine the number of layers of the lower-layer transition metal sulfide, the upper-layer transition metal sulfide and the isolation layer.
According to the method for testing the defect influence energy transfer in the two-dimensional material heterojunction, the isolation layer comprises a plurality of layers of boron nitride.
According to the method for testing the influence of the defects in the two-dimensional material heterojunction on energy transfer, the lower-layer transition metal sulfide is tungsten disulfide, and the upper-layer transition metal sulfide is molybdenum disulfide.
According to the invention, the method for testing the defect influence energy transfer in the two-dimensional material heterojunction is provided, and the plasma treatment comprises the following steps:
and placing the heterojunction into an oxygen plasma cavity for processing.
According to the method for testing the defect influence energy transfer in the two-dimensional material heterojunction, the detection of the heterojunction through the transient fluorescence lifetime imaging technology comprises the following steps:
the heterojunction was detected by an inverted fluorescence microscope with time-dependent single photon counting.
According to the method for testing the defect influence energy transfer in the two-dimensional material heterojunction, the detection of the heterojunction through the steady-state fluorescence spectrum technology comprises the following steps:
the heterojunction is detected by confocal raman spectroscopy.
According to the method for testing the influence of the defects in the two-dimensional material heterojunction on energy transfer, the isolation layer is arranged, so that a space can be formed between the lower transition metal sulfide and the upper transition metal sulfide, and the influence of charge transfer generated between the lower transition metal sulfide and the upper transition metal sulfide on the accuracy of a test result is avoided. And detecting the heterojunction after introducing the defects into the heterojunction through plasma treatment, and comparing the detection results of the heterojunction at different treatment times to obtain the influence of the defects with different densities on the energy transfer of the heterojunction.
Drawings
In order to more clearly illustrate the technical solutions of the present invention or the prior art, the drawings needed for the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart of a method for testing the effect of defects on energy transfer in a two-dimensional material heterojunction according to the present invention;
figure 2 is an optical microscope image of a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction provided by the present invention;
FIG. 3 is a Raman spectrum of molybdenum disulfide in a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction with plasma treatment at different times as provided by the present invention;
FIG. 4 is a plot of the steady state PL spectral intensity of a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction at various times during plasma processing as provided by the present invention;
FIG. 5 is a graph of the fluorescence lifetime of a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction at different times of plasma treatment provided by the present invention;
FIG. 6 is a graph of time-resolved fluorescence lifetime decay for different regions in a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction processed at different times by a plasma provided by the present invention;
fig. 7 is a graph of energy transfer rate and energy transfer efficiency provided by the present invention as a function of plasma processing time.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The method for testing the defect influence energy transfer in the two-dimensional material heterojunction according to the invention is described below with reference to fig. 1 to 7.
Specifically, the method for testing the influence of defects in a two-dimensional material heterojunction on energy transfer comprises the following steps:
a single-layer lower transition metal sulfide, an isolation layer and a single-layer upper transition metal sulfide are sequentially arranged from bottom to top to prepare the heterojunction.
The heterojunction is subjected to several plasma treatments to introduce defects into the heterojunction, and the first treatment time is 0 seconds.
And detecting the heterojunction after the heterojunction is subjected to plasma treatment every time.
The isolation layer is arranged, so that a gap is formed between the lower transition metal sulfide and the upper transition metal sulfide, and the influence of charge transfer between the lower transition metal sulfide and the upper transition metal sulfide on the accuracy of a test result is avoided. And detecting the heterojunction after introducing the defects into the heterojunction through plasma treatment, and comparing the detection results of the heterojunction at different treatment times to obtain the influence of the defects with different densities on the energy transfer of the heterojunction.
In some embodiments provided herein, detecting a heterojunction includes:
the heterojunction is detected by a steady state fluorescence spectroscopy technique to obtain a PL spectrum of the heterojunction for a corresponding processing time.
And/or detecting the heterojunction through a transient fluorescence lifetime imaging technology to obtain a fluorescence lifetime imaging graph and a fluorescence lifetime attenuation curve of the heterojunction at corresponding processing time.
After the defects are introduced into the heterojunction through plasma treatment, the heterojunction is detected through a steady-state fluorescence spectrum technology and a transient fluorescence lifetime imaging technology, and the influence of the defects on the energy transfer of the heterojunction can be obtained by comparing the detection results of the heterojunction at different treatment times. And the influence of the defects on the energy transfer can be rapidly and intuitively observed through the steady-state fluorescence spectrum and the transient fluorescence lifetime imaging graph.
In some embodiments provided herein, the lower transition metal sulfide is tungsten disulfide and the upper transition metal sulfide is molybdenum disulfide.
In some embodiments provided herein, the isolation layer comprises a number of layers of boron nitride. The boron nitride can prevent charge transfer between the lower transition metal sulfide and the upper transition metal sulfide. Alternatively, the number of layers of boron nitride is set to 10 to 20.
The following description will be given by taking tungsten disulfide as a transition metal sulfide of the lower layer and molybdenum disulfide as a transition metal sulfide of the upper layer as an example. The heterojunction of the rest of the materials has the same principle.
Optionally, the above sequentially placing a single layer of lower transition metal sulfide, an isolation layer, and a single layer of upper transition metal sulfide from bottom to top to prepare a heterojunction includes:
firstly, preparing a single-layer molybdenum disulfide, tungsten disulfide and a plurality of layers of boron nitride samples by adopting a mechanical stripping method. A single layer of tungsten disulfide is mechanically stripped from the bulk crystal onto the glass substrate, while a single layer of molybdenum disulfide and several layers of boron nitride are mechanically stripped from the bulk crystal onto the gel film substrate. Under an optical microscope, a plurality of layers of boron nitride on the gel film substrate are covered on a single layer of tungsten disulfide, and after covering and contacting, the mixture is kept stand for 5 minutes to obtain a boron nitride/tungsten disulfide heterojunction. And covering the molybdenum disulfide of the gel film substrate on the boron nitride/tungsten disulfide heterojunction on the glass substrate again, and finally obtaining the molybdenum disulfide/boron nitride/tungsten disulfide heterojunction on the glass substrate.
Refer to the raman spectra of molybdenum disulfide in a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction for different times of plasma treatment as shown in figure 3. Raman characteristic peak surface A of molybdenum disulfide1gThe modes appear blue-shifted and in-plane
The pattern exhibited a more pronounced red shift with increasing oxygen plasma exposure time, indicating that defects were introduced into the molybdenum disulfide after plasma treatment and that the defect density increased with increasing plasma treatment time.
The PL spectra of a single layer of tungsten disulfide and a single layer of molybdenum disulfide were measured and compared to the PL spectra of a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction with a plasma treatment time of 0 second. Compared with a single-layer structure of a corresponding material, the PL intensity of the tungsten disulfide layer in the molybdenum disulfide/boron nitride/tungsten disulfide heterojunction region with the plasma processing time of 0 second is enhanced, the PL intensity of the molybdenum disulfide layer is greatly reduced, the PL peak value is not obviously changed, the defect-free molybdenum disulfide/boron nitride/tungsten disulfide heterojunction can be obtained, the energy transfer process exists, and the energy is transferred from the molybdenum disulfide layer to the tungsten disulfide layer.
Refer to the steady state PL spectrum intensity plot of the molybdenum disulfide/boron nitride/tungsten disulfide heterojunction at different times of plasma treatment as shown in figure 4. The influence of different defect densities on the energy transfer of the molybdenum disulfide/boron nitride/tungsten disulfide heterojunction can be obtained. Defects may facilitate more energy transfer.
Comparing PL spectra of molybdenum disulfide/boron nitride/tungsten disulfide heterojunctions at different processing times, it is found that PL intensity of tungsten disulfide in the molybdenum disulfide/boron nitride/tungsten disulfide heterojunctions increases with increasing plasma processing time, energy transfer in defect-enhanced molybdenum disulfide/boron nitride/tungsten disulfide heterojunctions can be obtained, and in a certain range, energy transfer efficiency increases with increasing defect density.
Refer to figure 5 for a graph of the fluorescence lifetime of a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction imaged at different times during plasma processing. The influence of defects with different densities on the energy transfer of the molybdenum disulfide/boron nitride/tungsten disulfide heterojunction can be obtained. Defects can accelerate more energy transfer and exciton recombination time is shortened.
The reduction of exciton decay time in a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction region along with the increase of plasma treatment time can be visually monitored through a fluorescence lifetime imaging graph, the defect acceleration of energy transfer in the molybdenum disulfide/boron nitride/tungsten disulfide heterojunction can be obtained, and in a certain range, the energy transfer rate is increased along with the increase of defect density.
In some embodiments provided herein, detecting a heterojunction by a steady-state fluorescence spectroscopy technique comprises: the heterojunction was detected by confocal raman spectroscopy. For example, LabRAM HR Evolution type confocal Raman spectrometer.
In some embodiments provided herein, detecting heterojunctions by transient fluorescence lifetime imaging techniques comprises: heterojunctions were detected by an inverted fluorescence microscope with time-dependent single photon counting. For example, an inverted fluorescence microscope model IX83, manufactured by Olympus, may be used.
In some embodiments provided by the present invention, after obtaining the fluorescence lifetime decay curve of the heterojunction at the corresponding processing time, the method further comprises:
fitting a fluorescence lifetime decay curve to obtain exciton lifetime and average exciton lifetime;
the energy transfer rate and energy transfer efficiency were calculated from the average exciton lifetime.
In particular, a double exponential function may be used:
fitting the fluorescence lifetime decay curve to obtain A1、A2、τ1And τ2. Wherein A is1And A2To normalize the amplitude component, τ1And τ2The exciton lifetime.
It is noted that the step of fitting the fluorescence lifetime decay curve may be performed by an inverted fluorescence microscope, wherein A1、A2、τ1And τ2All can be obtained from an inverted fluorescence microscope.
According to A1、A2、τ1And τ2And based on the lifetime formula:
τav＝A1τ1+A2τ2
the average exciton lifetime τ can be obtainedav。
From the lifetime formula above, and the normalized amplitude component and exciton lifetime in the heterojunction read from the inverted fluorescence microscope, the average exciton lifetime τ of the heterojunction can be calculatedheter. From the lifetime formula above, and the normalized amplitude component of the donor and exciton lifetime read from the inverted fluorescence microscope, the average exciton lifetime τ of the donor can be calculateddonor. For a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction, the donor refers to the molybdenum disulfide layer. As shown in fig. 5, τdonorCan also be directly obtained in the molybdenum disulfide layer region in a fluorescence lifetime imaging graph generated by an inverted fluorescence microscopeAnd (6) taking. Selecting a molybdenum disulfide layer region in a fluorescence lifetime imaging graph, deconvoluting (considering instrument response) and fitting with double indexes, and calculating the average exciton lifetime to obtain taudonor。τheterOr directly obtaining the molybdenum disulfide/boron nitride/tungsten disulfide heterojunction region in a fluorescence lifetime imaging graph generated by an inverted fluorescence microscope. Selecting a molybdenum disulfide/boron nitride/tungsten disulfide heterojunction region in a fluorescence lifetime imaging graph, deconvoluting (considering instrument response) and fitting with double indexes, and calculating the average exciton lifetime to obtain tauheter。
According to τheterAnd τdonorBased on the energy transfer rate formula:
1/τET＝1/τheter-1/τdonor
the energy transfer rate can be calculated.
According to τheterAnd τdonorBased on the energy transfer efficiency formula:
ηET＝1-τheter/τdonor
the energy transfer efficiency can be calculated.
Compared with the energy transfer rate and the energy transfer efficiency of the heterojunction with different processing time, the influence of the defects with different densities in the heterojunction on the energy transfer rate and the energy transfer efficiency can be obtained quantitatively.
Referring to fig. 7, a graph of energy transfer rate and energy transfer efficiency as a function of plasma processing time is shown. The energy transfer efficiency and the energy transfer rate increase with an increase in defect density.
In some embodiments provided by the present invention, before performing the plasma treatment on the heterojunction for several times, the method further comprises:
and respectively checking the lower transition metal sulfide and the upper transition metal sulfide through the steady-state Raman spectrum characteristic peak value and the characteristic peak value difference. Because different transition metal sulfides show different characteristic peaks and characteristic peak differences, the sample information of the transition metal sulfides can be verified through a steady-state Raman spectrum.
Therefore, the sample information of the lower transition metal sulfide and the upper transition metal sulfide adopted in the test process can be verified, and the adoption of wrong materials is avoided.
Further, the steady state raman spectrum can also be collected using a confocal raman spectrometer as described above.
In some embodiments provided by the present invention, before performing the plasma treatment on the heterojunction for several times, the method further comprises:
and respectively detecting the thicknesses of the lower transition metal sulfide, the upper transition metal sulfide and the isolating layer of the heterojunction to determine the number of layers of the lower transition metal sulfide, the upper transition metal sulfide and the isolating layer.
Therefore, whether the number of layers of the lower-layer transition metal sulfide, the upper-layer transition metal sulfide and the isolation layer adopted in the test process is correct can be verified. Further, the thicknesses of the lower transition metal sulfide, the upper transition metal sulfide and the isolation layer of the heterojunction can be tested by adopting an atomic force microscope.
In some embodiments provided herein, the plasma treatment comprises: the heterojunction is placed in an oxygen plasma chamber for processing. For example, the sample may be processed in a 10W oxygen plasma chamber at a radio frequency of 13.56 MHz.
Further, each time the heterojunction is plasma treated, the time is greater than zero seconds, but is virtually additive with regard to heterojunction-induced defects. For example, when the first time of plasma treatment of the heterojunction is 10 seconds, and after the correlation detection is performed, the second time of plasma treatment of the heterojunction is 5 seconds, the second time of plasma treatment is substantially 15 seconds after the second time of plasma treatment. Longer processing times indicate a greater defect density within the heterojunction.
Optionally, in order to improve the precision of the test, after performing plasma processing on the heterojunction every time, the heterojunction is detected within 5min, and after the test is finished, the heterojunction is placed into the plasma cavity again to perform plasma processing for the next time to be detected next time.
For example, the time for the heterojunction plasma treatment may be set to 0s, 10s, 20s, 30s, 35s, 40s, 48s, 56s, 64s, 72 s. The three treatments are described as an example, and the first treatment time is 0 s. The second processing time 10s is added to the first processing time, and then 10s is processed. The third treatment time 10s is added to the previous two treatment times to obtain a treatment time of 20 s.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for testing defects in a two-dimensional material heterojunction for affecting energy transfer, comprising:
placing a single-layer lower-layer transition metal sulfide, an isolation layer and a single-layer upper-layer transition metal sulfide in sequence from bottom to top to prepare a heterojunction;
carrying out plasma treatment on the heterojunction for several times to introduce defects into the heterojunction, wherein the first treatment time is 0 second;
and detecting the heterojunction after the heterojunction is subjected to plasma treatment every time.
2. The method of testing defect-affected energy transfer in a two-dimensional material heterojunction as claimed in claim 1 wherein said inspecting said heterojunction comprises:
detecting the heterojunction by a steady state fluorescence spectroscopy technique to obtain a PL spectrum of the heterojunction for a corresponding processing time; and/or the presence of a gas in the gas,
and detecting the heterojunction by a transient fluorescence lifetime imaging technology to obtain a fluorescence lifetime imaging graph and a fluorescence lifetime attenuation curve of the heterojunction at corresponding processing time.
3. The method for testing defect-affected energy transfer in a two-dimensional material heterojunction as claimed in claim 2, further comprising, after said obtaining the fluorescence lifetime decay curves of the heterojunction for respective processing times:
fitting the fluorescence lifetime decay curve to obtain exciton lifetime and average exciton lifetime;
calculating an energy transfer rate and an energy transfer efficiency from the average exciton lifetime.
4. The method of testing defect-affected energy transfer in a two-dimensional material heterojunction as claimed in claim 1, further comprising, prior to said subjecting said heterojunction to a number of plasma treatments:
and respectively verifying the lower-layer transition metal sulfide and the upper-layer transition metal sulfide through a steady-state Raman spectrum characteristic peak value and a characteristic peak value difference.
5. The method of testing defect-affected energy transfer in a two-dimensional material heterojunction as claimed in claim 1, further comprising, prior to said subjecting said heterojunction to a number of plasma treatments:
and respectively detecting the thicknesses of the lower-layer transition metal sulfide, the upper-layer transition metal sulfide and the isolation layer of the heterojunction to determine the number of layers of the lower-layer transition metal sulfide, the upper-layer transition metal sulfide and the isolation layer.
6. The method of testing for defect-affected energy transfer in a two-dimensional material heterojunction as claimed in claim 1 wherein said spacer layer comprises a plurality of layers of boron nitride.
7. The method for testing the influence of defects on energy transfer in a two-dimensional material heterojunction as claimed in claim 1, wherein the lower transition metal sulfide is tungsten disulfide and the upper transition metal sulfide is molybdenum disulfide.
8. The method of testing for defect-affected energy transfer in a two-dimensional material heterojunction as claimed in claim 1 wherein said plasma treatment comprises:
and placing the heterojunction into an oxygen plasma cavity for processing.
9. The method of claim 2, wherein the detecting the heterojunction by transient fluorescence lifetime imaging technique comprises:
the heterojunction was detected by an inverted fluorescence microscope with time-dependent single photon counting.
10. The method of claim 2, wherein the detecting the heterojunction by a steady state fluorescence spectroscopy technique comprises:
the heterojunction is detected by confocal raman spectroscopy.
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