CN104789219A - Molecular modification method capable of improving luminous efficiency of single-layer MoS2 - Google Patents

Molecular modification method capable of improving luminous efficiency of single-layer MoS2 Download PDF

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CN104789219A
CN104789219A CN201510206364.XA CN201510206364A CN104789219A CN 104789219 A CN104789219 A CN 104789219A CN 201510206364 A CN201510206364 A CN 201510206364A CN 104789219 A CN104789219 A CN 104789219A
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luminous efficiency
individual layer
molecular modification
toluene
mos
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CN104789219B (en
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苏伟涛
豆红雷
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Hangzhou Dianzi University
Hangzhou Electronic Science and Technology University
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Hangzhou Electronic Science and Technology University
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Abstract

The invention discloses a molecular modification method capable of improving luminous efficiency of single-layer MoS2, and in particular relates to a method capable of improving luminous efficiency of single-layer MoS2 by virtue of organic molecular modification. By virtue of a toluene/ethanol solution, a MoS2 sample prepared through micro-mechanical exfoliation is modified so as to obtain a molecular modified single-layer MoS2 sample. The morphology, the optical properties and the like of the modified sample are tested and analyzed by virtue of a metallurgical microscope, a Raman spectrometer, an atomic force microscope and the like. For the method disclosed by the invention, by carrying out molecular modification on the single-layer MoS2, the luminous efficiency of the single-layer MoS2 can be improved by 31.59 times. As reported before, through a complex annealing process under a vacuum environment, the effect of controlling gas pressure is enhanced by 35 times, while the vacuum annealing process is complex in technology and is instable in enhancing effect. Compared with the annealing process, the method disclosed by the invention has the advantages of significant effect of enhancing the luminous efficiency, simple experimental operation, strong feasibility, short preparation cycle, low cost, and operation at room temperature, and is free from toxicity and pollution.

Description

A kind of raising individual layer MoS 2the molecular modification method of luminous efficiency
Technical field
The invention belongs to field of material technology, be specifically related to a kind of raising individual layer MoS 2the molecular modification method of luminous efficiency.
Background technology
Individual layer MoS 2it is the material of a kind Graphene.Individual layer MoS 2be a kind of novelty, thickness in monolayer is 0.65nm and has the semiconductor material that direct band gap is about 1.8eV.Transient metal sulfide MoS 2there is electricity, optics and catalyst property and important dry lubricating performance, the application of Graphene can also be assisted, as: photoelectronics and energy storage.Individual layer MoS 2be direct band-gap semicondictor material, because it is the semi-conductor of atomic layer level thickness, therefore environment has suitable susceptibility to external world.By research individual layer MoS 2physical properties, to electron device of future generation, optics, biosensor development have important meaning.
Individual layer MoS 2be the semiconductor material of direct band gap, but himself luminous efficiency only has 0.5%, luminous efficiency is very low, and practical value is very low.
Summary of the invention
The object of this invention is to provide a kind of raising individual layer MoS 2the method of luminous efficiency, the method utilizes organic molecule modified monolayer MoS 2, realize improving individual layer MoS 2luminous efficiency.
The inventive method is:
Step (1), to SiO 2(280 ~ 300nm)/Si substrate carries out pre-treatment: utilize the organic molecule having strong oxidizing property compound solution removing substrate surface and may exist, specifically:
1.1 by SiO 2(280 ~ 300nm)/Si sheet cuts into 1 ~ 2cm 2square fritter is as substrate;
Under 1.2 normal temperature with deionized water by above-mentioned substrate ultrasonic cleaning 10 ~ 20 minutes;
Under 1.3 normal temperature with dehydrated alcohol by above-mentioned substrate ultrasonic cleaning 10 ~ 20 minutes;
Under 1.4 normal temperature with deionized water by above-mentioned substrate ultrasonic cleaning 10 ~ 20 minutes;
With there is strong oxidizing property compound solution by above-mentioned substrate ultrasonic cleaning 10 ~ 20 minutes under 1.5 normal temperature;
Under 1.6 normal temperature with deionized water by above-mentioned substrate ultrasonic cleaning 10 ~ 20 minutes, finally dry up;
Described strong oxidizing property compound can be hydrogen peroxide; Being preferably massfraction is 20 ~ 30% superoxols;
Step (2), micromechanics stripping means is adopted to obtain MoS2 sample to the pretreated substrate of step (1);
Step (3), be 1.007 × 10 by concentration -3~ 1.005 × 10 -9the toluene ethanolic soln of mol/L is evenly coated in MoS 2sample surfaces, or by above-mentioned MoS 2sample is dipped in toluene ethanolic soln and adopts crystal pulling method, obtains the finished product;
Described even coating method can be adopt sol evenning machine that toluene ethanolic soln is spin-coated on MoS2 sample surfaces, and sol evenning machine rotating speed is set to low speed 1000 ~ 2000 revs/min, and 8000 ~ 9000 revs/min at a high speed, spin-coating time is 10 ~ 40 seconds;
As preferably, described toluene ethanol solution concentration is 1.007 × 10 -3mol/L, 1.006 × 10 -6mol/L or 1.005 × 10 -9mol/L; More preferably 1.006 × 10 -6mol/L.
The product that test aforesaid method prepares can use the Raman spectrometer that excitation wavelength is 532nm to record individual layer MoS 2raman spectrum and PL spectrum.AFM tests.
The inventive method is by organic molecule (i.e. toluene) modified monolayer MoS 2, the individual layer MoS that the organic molecule prepared is modified 2luminous efficiency realizes raising 31.59 times.There is other method before this by complicated annealing process, under vacuum unit, control the reinforced effects that gas pressure intensity obtains 35 times.Once pressure change, its reinforced effects changes thereupon, and reinforced effects is unstable.The inventive method compare than, have luminous efficiency reinforced effects obvious, experimental implementation is simple, and feasibility is strong, and preparation cycle is short, and cost is low, at room temperature operates, the advantage of nontoxic pollution-free.
Accompanying drawing explanation
Fig. 1 is unadulterated individual layer MoS 2optics picture;
Fig. 2 is the toluene substance withdrawl syndrome that do not adulterate and adulterate is 1.007 × 10 -3the individual layer MoS of mol/L 2raman composes;
Fig. 3 is the toluene substance withdrawl syndrome that do not adulterate and adulterate is 1.007 × 10 -3the individual layer MoS of mol/L 2pL composes;
Fig. 4 is doping toluene substance withdrawl syndrome is 1.007 × 10 -3the individual layer MoS of mol/L 2optical photograph;
Fig. 5 is the toluene substance withdrawl syndrome that do not adulterate and adulterate is 1.006 × 10 -6the individual layer MoS of mol/L 2raman composes;
Fig. 6 is the toluene substance withdrawl syndrome that do not adulterate and adulterate is 1.006 × 10 -6the individual layer MoS of mol/L 2pL composes;
Fig. 7 is doping toluene substance withdrawl syndrome is 1.006 × 10 -6the individual layer MoS of mol/L 2optics picture;
Fig. 8 is the individual layer MoS that do not adulterate 2aFM schemes;
Fig. 9 is doping toluene substance withdrawl syndrome is 1.006 × 10 -6the individual layer MoS of mol/L 2aFM schemes;
Figure 10 is the toluene substance withdrawl syndrome that do not adulterate and adulterate is 1.005 × 10 -9the individual layer MoS of mol/L 2raman composes;
Figure 11 is the toluene substance withdrawl syndrome that do not adulterate and adulterate is 1.005 × 10 -9the individual layer MoS of mol/L 2pL composes;
Figure 12 is doping toluene substance withdrawl syndrome is 1.005 × 10 -9the individual layer MoS of mol/L 2optics picture.
Embodiment
For further analysis to the present invention below in conjunction with specific embodiments and the drawings.
Embodiment 1.
Step (1). getting purity is AR, and the toluene of 99.5% and purity are AR, the dehydrated alcohol of 99.7%, and it is 1.007 × 10 that preparation obtains substance withdrawl syndrome -3mol/L toluene ethanolic soln.
Step (2). by SiO 2(300nm)/Si sheet cuts into 1cm 2square fritter is as substrate.
Step (3). under room temperature with deionized water by step (2) gained substrate ultrasonic cleaning 10 minutes.
Step (4). with AR under room temperature, the ethanol solution of 99.7% was by step (3) gained substrate ultrasonic cleaning 10 minutes.
Step (5). under room temperature with deionized water by step (4) gained substrate ultrasonic cleaning 10 minutes.
Step (6). be 30% hydrogen peroxide by step (5) gained substrate ultrasonic cleaning 10 minutes with massfraction under room temperature.
Step (7). under room temperature with deionized water by step (6) gained substrate ultrasonic cleaning 10 minutes.
Step (8). dry up step (7) gained substrate, the method using micromechanics to peel off obtains MoS 2sample.
Step (9). sol evenning machine rotating speed is set to low speed 1000 revs/min, 8000 revs/min at a high speed, controlling spin-coating time is low speed 10 seconds, 30 seconds at a high speed.Be 1.007 × 10 by step (1) gained substance withdrawl syndrome -3the toluene ethanolic soln of mol/L is spin-coated on the sample of step (8) gained.Sample preparation completes.
Step (10). test procedure (9) gained sample, uses the Raman spectrometer that excitation wavelength is 532nm to record individual layer MoS 2raman spectrum and PL spectrum.AFM tests.
Be illustrated in figure 1 the individual layer MoS that do not adulterate 2optics picture is the toluene substance withdrawl syndrome that do not adulterate and adulterate shown in Fig. 2 is 1.007 × 10 -3the individual layer MoS of mol/L 2raman composes, and right side peak position moves 2.979cm -1, be the doping of P type.Be the toluene substance withdrawl syndrome that do not adulterate and adulterate shown in Fig. 3 be 1.007 × 10 -3the individual layer MoS of mol/L 2pL composes, and luminous efficiency improves 4.56 times.Be doping toluene substance withdrawl syndrome shown in Fig. 4 be 1.007 × 10 -3the individual layer MoS of mol/L 2optical photograph.
Embodiment 2.
Step (1). getting purity is AR, and the toluene of 99.5% and purity are AR, the dehydrated alcohol of 99.7%, and it is 1.006 × 10 that preparation obtains substance withdrawl syndrome -6mol/L toluene solution.
Step (2). by SiO 2(280nm)/Si sheet cuts into 2cm 2square fritter is as substrate.
Step (3). under room temperature with deionized water by step (2) gained substrate ultrasonic cleaning 20 minutes.
Step (4). with AR under room temperature, the ethanol solution of 99.7% was by step (3) gained substrate ultrasonic cleaning 20 minutes.
Step (5). under room temperature with deionized water by step (4) gained substrate ultrasonic cleaning 20 minutes.
Step (6). be 20% hydrogen peroxide by step (5) gained substrate ultrasonic cleaning 20 minutes with massfraction under room temperature.
Step (7). under room temperature with deionized water by step (6) gained substrate ultrasonic cleaning 20 minutes.
Step (8). dry up step (7) gained substrate, the method using micromechanics to peel off obtains MoS 2sample.
Step (9). sol evenning machine rotating speed is set to low speed 2000 revs/min, 9000 revs/min at a high speed, controlling spin-coating time is low speed 3 seconds, 7 seconds at a high speed.Be 1.006 × 10 by step (1) gained substance withdrawl syndrome -6the toluene solution of mol/L is spin-coated on the sample of step (8) gained.Sample preparation completes.
Step (10). test procedure (9) gained sample, uses the Raman spectrometer that excitation wavelength is 532nm to record individual layer MoS 2raman spectrum and PL spectrum.AFM tests.
Be the toluene substance withdrawl syndrome that do not adulterate and adulterate as shown in Figure 5 be 1.006 × 10 -6the individual layer MoS of mol/L 2raman composes, and right side peak position moves 2.143cm -1, be the doping of P type.Be the toluene substance withdrawl syndrome that do not adulterate and adulterate shown in Fig. 6 be 1.006 × 10 -6the individual layer MoS of mol/L 2pL composes, and luminous efficiency improves 31.59 times.Be doping toluene substance withdrawl syndrome shown in Fig. 7 be 1.006 × 10 -6the individual layer MoS of mol/L 2optical photograph.Fig. 8 is the individual layer MoS that do not adulterate 2aFM picture.Fig. 9 is doping toluene substance withdrawl syndrome is 1.006 × 10 -6the individual layer MoS of mol/L 2aFM picture.
Embodiment 3.
Step (1). getting purity is AR, and the toluene of 99.5% and purity are AR, the dehydrated alcohol of 99.7%, and it is 1.005 × 10 that preparation obtains substance withdrawl syndrome -9mol/L toluene solution.
Step (2). by SiO 2(290nm)/Si sheet cuts into 1cm 2square fritter is as substrate.
Step (3). under room temperature with deionized water by step (2) gained substrate ultrasonic cleaning 15 minutes.
Step (4). with AR under room temperature, the ethanol solution of 99.7% was by step (3) gained substrate ultrasonic cleaning 15 minutes.
Step (5). under room temperature with deionized water by step (4) gained substrate ultrasonic cleaning 15 minutes.
Step (6). be 20% hydrogen peroxide by step (5) gained substrate ultrasonic cleaning 20 minutes with massfraction under room temperature.
Step (7). under room temperature with deionized water by step (6) gained substrate ultrasonic cleaning 20 minutes.
Step (8). dry up step (7) gained substrate, use micromechanics stripping method to obtain MoS 2sample.
Step (9). sol evenning machine rotating speed is set to low speed 1500 revs/min, 8500 revs/min at a high speed, controlling spin-coating time is low speed 10 seconds, 15 seconds at a high speed.Be 1.005 × 10 by step (1) gained substance withdrawl syndrome -9the toluene solution of mol/L is spin-coated on the sample of step (8) gained.Sample preparation completes.
Step (10). test procedure (9) gained sample, uses the Raman spectrometer that excitation wavelength is 532nm to record individual layer MoS 2raman spectrum and PL spectrum.AFM tests.
Be the toluene substance withdrawl syndrome that do not adulterate and adulterate as shown in Figure 10 be 1.005 × 10 -9the individual layer MoS of mol/L 2raman composes, and right side peak position moves 1.351cm -1, be the doping of P type.Be the toluene substance withdrawl syndrome that do not adulterate and adulterate shown in Figure 11 be 1.005 × 10 -9the individual layer MoS of mol/L 2pL composes, and luminous efficiency improves 4.32 times.Be doping toluene substance withdrawl syndrome shown in Figure 12 be 1.005 × 10 -9the individual layer MoS of mol/L 2optical photograph.

Claims (7)

1. one kind is improved individual layer MoS 2the molecular modification method of luminous efficiency, is characterized in that the method comprises the following steps:
Step (1), to SiO 2(280 ~ 300nm)/Si substrate carries out pre-treatment: utilize the organic molecule having strong oxidizing property compound solution removing substrate surface and may exist;
Step (2), micromechanics stripping means is adopted to the pretreated substrate of step (1) or obtains MoS 2sample;
Step (3), be 1.007 × 10 by concentration -3~ 1.005 × 10 -9the toluene ethanolic soln of mol/L is evenly coated in MoS 2sample surfaces, or by above-mentioned MoS 2sample is dipped in toluene ethanolic soln and adopts crystal pulling method, obtains the finished product.
2. a kind of raising individual layer MoS as claimed in claim 1 2the molecular modification method of luminous efficiency, is characterized in that step (1) concrete operations are:
1.1 by SiO 2(280 ~ 300nm)/Si sheet cuts into 1 ~ 2cm 2square fritter is as substrate;
Under 1.2 normal temperature with deionized water by above-mentioned substrate ultrasonic cleaning 10 ~ 20 minutes;
Under 1.3 normal temperature with dehydrated alcohol by above-mentioned substrate ultrasonic cleaning 10 ~ 20 minutes;
Under 1.4 normal temperature with deionized water by above-mentioned substrate ultrasonic cleaning 10 ~ 20 minutes;
With there is strong oxidizing property compound solution by above-mentioned substrate ultrasonic cleaning 10 ~ 20 minutes under 1.5 normal temperature;
Under 1.6 normal temperature with deionized water by above-mentioned substrate ultrasonic cleaning 10 ~ 20 minutes, finally dry up.
3. a kind of molecular modification method improving individual layer MoS2 luminous efficiency as claimed in claim 1 or 2, is characterized in that the strong oxidizing property compound described in step (1) is hydrogen peroxide.
4. a kind of molecular modification method improving individual layer MoS2 luminous efficiency as claimed in claim 1 or 2, the strong oxidizing property compound that it is characterized in that described in step (1) is massfraction is 20 ~ 30% superoxols.
5. a kind of molecular modification method improving individual layer MoS2 luminous efficiency as claimed in claim 1 or 2 or 3 or 4, is characterized in that the toluene ethanol solution concentration described in step (3) is 1.007 × 10-3mol/L, 1.006 × 10-6mol/L or 1.005 × 10-9mol/L.
6. one as claimed in claim 1 or 2 or 3 or 4 improves individual layer MoS 2the molecular modification method of luminous efficiency, is characterized in that the toluene ethanol solution concentration described in step (3) is 1.006 × 10 -6mol/L.
7. the one as described in claim 1 or 2 or 3 or 4 or 5 or 6 improves individual layer MoS 2the molecular modification method of luminous efficiency, it is characterized in that the even coating method described in step (3) can be adopt sol evenning machine that toluene ethanolic soln is spin-coated on MoS2 sample surfaces, sol evenning machine rotating speed is set to low speed 1000 ~ 2000 revs/min, 8000 ~ 9000 revs/min at a high speed, spin-coating time is 10 ~ 40 seconds.
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CN105648403A (en) * 2016-01-04 2016-06-08 山东师范大学 MoS2/Cu nanometer particle SERS substrate and preparing method thereof
CN109449244A (en) * 2018-10-22 2019-03-08 中国科学院上海技术物理研究所 A kind of two-dimensional semiconductor and ferroelectric material have complementary functions type ultra-wide spectrum detector
CN113451139A (en) * 2021-06-23 2021-09-28 复旦大学 Method for carrying out p-type doping on TMDCs based on PTFE and semiconductor

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105648403A (en) * 2016-01-04 2016-06-08 山东师范大学 MoS2/Cu nanometer particle SERS substrate and preparing method thereof
CN109449244A (en) * 2018-10-22 2019-03-08 中国科学院上海技术物理研究所 A kind of two-dimensional semiconductor and ferroelectric material have complementary functions type ultra-wide spectrum detector
CN109449244B (en) * 2018-10-22 2020-06-26 中国科学院上海技术物理研究所 Two-dimensional semiconductor and ferroelectric material function complementary type ultra-wide spectrum detector
CN113451139A (en) * 2021-06-23 2021-09-28 复旦大学 Method for carrying out p-type doping on TMDCs based on PTFE and semiconductor

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