CN107328754B - Photoelectric synergistic surface plasmon-exciton catalytic reaction device and preparation method thereof - Google Patents
Photoelectric synergistic surface plasmon-exciton catalytic reaction device and preparation method thereof Download PDFInfo
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Abstract
The invention provides a photoelectric synergistic surface plasmon-exciton catalytic reaction device and a preparation method thereof, and belongs to the technical field of surface catalytic reaction devices. Firstly, thermally evaporating noble metal nano particles on a silicon slice of silicon dioxide/monocrystalline silicon, transferring a two-dimensional semiconductor material onto a noble metal nano particle substrate, and sequentially evaporating gold/chromium nano particles onto a two-dimensional semiconductor material and metal nano particle composite substrate as a source electrode/drain electrode in a thermal evaporation mode according to a chromium-first-and-gold-last sequence, wherein the sizes and gaps of the two electrodes are controllable; and finally, introducing a gate voltage at the bottom of the device by using the base. When the method is used for specifically manufacturing a device, the size of the shelter is convenient to control, so that the size of a gap between the source electrode and the drain electrode is controllable, gaps with different sizes can be designed according to the requirements of specific experiments, the available area of molecular reaction is improved, the local surface plasmon resonance effect is further improved, and the efficiency of surface catalysis reaction is improved.
Description
Technical Field
The invention relates to the technical field of surface catalytic reaction devices, in particular to a photoelectric synergistic surface plasmon-exciton catalytic reaction device and a preparation method thereof.
Background
Surface Plasmons (SPs) are resonance excitation elements formed by coherent coupling of electromagnetic waves (light) with quasi-free electron gas collective oscillation in a metal (or doped semiconductor) surface. Electronic oscillations that can be localized at the surface of metal nanoparticles are commonly referred to as Localized Surface Plasmon Resonance (LSPR). In the nanoscale, plasmon-induced catalytic reactions predominate, which we generally refer to as plasmon-induced chemical reactions. It is well known that hot electrons generated by plasmon decay play an important role in plasmon-induced chemical reactions. When the hot electrons are temporarily adsorbed to the target molecules, the neutral potential surface (PES) of the molecules in the plasmon-induced chemical reaction is injected with electrons, thus significantly lowering the reaction barrier of the molecules, while the hot electrons can also temporarily function as a linking molecule. Meanwhile, the kinetic energy of the hot electrons can be effectively transferred to target molecules to provide energy for catalytic reaction; hot electrons can also be used as the energy required for catalytic reactions to drive molecular reactions.
However, as can be seen from the data in document 1 (Langmuir, 2011;27[17]: 10677), the state density of hot electrons generated by plasmon decay is very low, and the lifetime is short, and thus the efficiency of the plasmon-induced surface catalytic reaction is relatively low. To overcome these drawbacks, the advent of surface plasmon-exciton coupling interactions provides a new concept because the presence of excitons, the hot electrons generated by the coupling system accumulate more easily and their lifetime is greatly increased from femtoseconds to picoseconds compared to plasmon-only. On the other hand, the local surface plasmon resonance effect can greatly enhance the local electromagnetic field, so that the generation of excitons can be further promoted, and the efficiency of catalytic reaction is increased. In summary, the efficiency of the plasmon-exciton coupled co-driven surface catalytic reaction is much higher than that induced by surface plasmons alone.
However, the methods of exciton introduction that are common today are mainly by photoinduction. As reported in document 2 (Materials Today Energy,2017; 5:72), photoinduced excitons are coupled with plasmons by interaction of laser light and a two-dimensional semiconductor material, thereby driving the progress of a surface catalytic reaction.
The design of the common electrical devices is mainly limited to micro-nano size, as reported in document 3 (Nature, 2008; 451:163), the observable range is small, the processing difficulty is high, the cost is high, and the commonly used Raman scattering spectrum instrument is difficult to accurately position.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a photoelectric synergistic surface plasmon-exciton catalytic reaction device and a preparation method thereof, so that the electric field effect is introduced while the optical field is used for regulating and controlling the surface plasmon-exciton coupling catalytic reaction, and the design of the device can be improved, so that the catalytic reaction can be carried out more cheaply and effectively.
The device comprises a silicon wafer, a two-dimensional semiconductor material and a source electrode/drain electrode, wherein noble metal nano particles are covered on the silicon wafer, the two-dimensional semiconductor material is covered on the noble metal nano particles, the source electrode/drain electrode is positioned on the two-dimensional semiconductor material, the silicon wafer is arranged on a base, and a gate voltage is introduced to the bottom of the base.
Wherein the silicon wafer comprises SiO 2 A layer and a Si layer covered with SiO 2 A layer.
The preparation method of the device comprises the following steps:
s1: thermally evaporating noble metal nano particles on a silicon slice of silicon dioxide/monocrystalline silicon to obtain a noble metal nano material substrate; according to the proper laser wavelength, metal nano particles with different thickness are deposited by a thermal evaporation method, for example, silver nano particles with the thickness of 10nm can be thermally evaporated by 532nm laser;
s2: transferring a two-dimensional semiconductor material onto the noble metal nanoparticle substrate prepared in the step S1, and cleaning to ensure surface cleaning;
s3: evaporating gold/chromium nano particles onto the two-dimensional semiconductor material and metal nano particle composite substrate prepared in the step S2 in a thermal evaporation mode according to the sequence of chromium first and gold later to serve as a source electrode/drain electrode;
s4: the gate voltage is introduced at the bottom of the device fabricated in S3 using the mount. (SiO on a silicon wafer in general) 2 The breakdown voltage of the layer is 110V).
Wherein the thickness of the noble metal nano-particles thermally evaporated in the S1 is 1-100nm.
The thickness of chromium in S3 is 5nm, and the thickness of gold is 80-100nm.
The size and the gap between the two electrodes of the source electrode and the drain electrode in the S3 can be adjusted, and the target molecule is positioned between the two electrodes.
The device of the invention can be used for the following determination:
(1) The device in the invention is used for measuring current diagrams of different gate voltages (-60V) and bias voltages (-1.0V);
(2) The device in the invention is used for measuring the Raman spectrum of the catalytic reaction process under different laser wavelengths (200 nm-1000 nm) and light intensities (5 uW-10 mW);
(3) The device of the invention is used for measuring a Raman spectrum of a surface catalytic reaction process driven by a bias voltage (-1.0V) under a certain fixed laser wavelength (200 nm-1000 nm) and a certain light intensity (5 uW-10 mW) and a certain fixed gate voltage (-60V);
(4) The device of the invention is used for measuring the Raman spectrum of the surface catalytic reaction process under different laser wavelengths (200 nm-1000 nm) and light intensities (5 uW-10 mW), different gate voltages (-60V) and bias voltages (-1.0V).
The technical scheme of the invention has the following beneficial effects:
(1) When a device is specifically manufactured, the size of the shelter is convenient to control, so that the size of a gap between the source electrode and the drain electrode is controllable, gaps with different sizes can be designed according to the requirements of specific experiments, the available area of molecular reaction is improved, the local surface plasmon resonance effect is further improved, and the efficiency of surface catalysis reaction is improved;
(2) As long as the two-dimensional semiconductor material is transferred properly, the size of the device is very easy to control, so that the manufacturing cost of the device is greatly reduced, and the electric field regulation and control are easier to introduce into a system;
(3) The structural design of the device is suitable for photoelectric cooperative regulation, and the regulation effect of an incident light source is not influenced when an electric field is introduced.
In addition, the photoelectric cooperative regulation surface plasmon-exciton coupling catalytic reaction has the following advantages:
(1) While ensuring that the laser regulation surface plasmon-exciton coupling catalytic reaction is not influenced, an electric field is introduced to regulate the surface plasmon-exciton coupling catalytic reaction, so that the regulatable parameters are greatly increased, and the driving modes of the surface catalytic reaction are diversified. Meanwhile, the electrical property of the device can be measured, so that the improvement of the surface catalytic reaction property is explained;
(2) The gate voltage is regulated, so that the Fermi surface of a coupling system of a two-dimensional semiconductor material (single-layer graphene and the like) and noble metal nano particles (silver, gold and the like) can be regulated, the state density of hot electrons is further improved, and the efficiency of surface catalytic reaction is improved;
(3) By adjusting bias voltage to generate current, the thermal electrons generated by the plasmons obtain larger kinetic energy, so that the surface catalytic reaction is promoted, and the catalytic efficiency is improved;
(4) Further facilitating the deep analysis of the physical principles of plasmon and exciton coupling action and the participation mechanism of electrons in catalytic reaction.
Drawings
FIG. 1 is a schematic diagram of a structure of a photoelectrocooperative surface plasmon-exciton catalytic reaction device of the present invention;
FIG. 2 is an electrical measurement diagram of a surface plasmon-exciton coupled catalytic reaction device of the present invention when target molecules (4 NBT) are not adsorbed and adsorbed, (a) is a 3D continuous graph of gate voltage and bias control current variation when target molecules (4 NBT) are not adsorbed, (b) is a 3D continuous graph of gate voltage and bias control current variation when target molecules (4 NBT) are adsorbed, (c) is a bias-current diagram of different gate voltages when target molecules (4 NBT) are not adsorbed, (D) is a bias-current diagram of different gate voltages when target molecules (4 NBT) are adsorbed, (e) is a bias voltage V when target molecules (4 NBT) are not adsorbed Bias Gate voltage-conductance diagram at=0.1v, (f) is adsorption target molecule (4 NBT) and bias V Bias Gate voltage-conductance plot at =0.1v;
FIG. 3 is a Raman spectrum of a surface catalytic reaction process on a surface plasmon-exciton coupling catalytic reaction device under different laser power modulation;
FIG. 4 is a Raman spectrum and schematic diagram (bias modulation) of a photoelectro-co-surface plasmon-exciton coupling catalytic reaction process, (a) a bias-modulated surface plasmon-exciton coupling catalytic reaction at a fixed laser power and a gate voltage of 0V, (b) a bias-modulated surface plasmon-exciton coupling catalytic reaction at a fixed laser power and a gate voltage of 40V, (c) a bias-modulated surface plasmon-exciton coupling catalytic reaction at a fixed laser intensity and a gate voltage of-40V, (d) a schematic diagram (bias modulation) of a photoelectro-co-surface plasmon-exciton coupling catalytic reaction, wherein white areas in triangles are holes and black filled areas are electrons;
FIG. 5 shows a Raman spectrum and a schematic diagram (gate voltage regulation) of a photoelectro-co-surface plasmon-exciton coupling catalytic reaction process, (a) shows a surface plasmon-exciton coupling catalytic reaction with a fixed laser power and a gate voltage regulation when a bias voltage is 0V, (b) shows a surface plasmon-exciton coupling catalytic reaction with a fixed laser power and a gate voltage regulation when a bias voltage is 1V, (c) shows a surface plasmon-exciton coupling catalytic reaction with a fixed laser intensity and a gate voltage regulation when a bias voltage is-1V, and (d) shows a schematic diagram (gate voltage regulation) of a photoelectro-co-surface plasmon-exciton coupling catalytic reaction, wherein white areas in triangles are holes and black filling areas are electrons.
Wherein: 1-incidence of laser light; 2-source/drain; 3-target molecule; 4-a two-dimensional semiconductor material; 5-silver nanoparticles; 6-SiO 2 A layer; 7-Si layer.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
The invention provides a photoelectric synergistic surface plasmon-exciton catalytic reaction device and a preparation method thereof.
1. Fabrication of a photoelectro-cooperative surface plasmon-exciton coupling catalytic reaction device:
1) Vacuum degree at room temperature was 8.6x10 -5 In the Pa environment by thermal evaporation
Is deposited on a silicon wafer with 300nm thick silicon dioxide at a rate of 10nm thick silver nanoparticles 5;
2) Spin-coating PMMA (3000 rpm,1 min) on copper-based single-layer graphene grown by CVD, putting into 0.5Mol/L ferric trichloride solution to corrode a substrate for more than 4 hours until copper base is removed, obtaining a two-dimensional semiconductor material 4, washing with deionized water for more than 4 times, transferring to a substrate with silver nano particles 5, and finally removing PMMA on the surface of the graphene with acetone;
3) After the single-layer graphene-silver nanoparticle substrate is cleaned and dried for many times, two electrodes of a source electrode/drain electrode 2 are added on two sides of the single-layer graphene-silver nanoparticle substrate by thermal evaporation, the gap between the two electrodes of the source electrode/drain electrode 2 is 60 micrometers, and the vacuum degree of precipitated metal is 1.10x10 -5 Pa. The method comprises the following specific steps: first a 60 micron wire is placed on a single layer of stoneOn a graphene-silver nanoparticle substrate, then in a form of
Is deposited at a rate of 5nm thick of chromium nanoparticles, finally +.>
A 90nm thick gold film was deposited. The design of the photoelectric synergistic surface plasmon-exciton coupling catalytic reaction device is shown in figure 1, incident laser 1 is arranged above the photoelectric synergistic surface plasmon-exciton coupling catalytic reaction device, target molecules 3 are arranged between a source electrode and a drain electrode 2, and silver nano particles 5 are thermally evaporated on SiO 2 On layer 6, siO 2 Below layer 6 is Si layer 7.
2. Measurement of photoelectrosynergistic surface plasmon-exciton coupling catalytic reaction:
1) In order to protect the target molecules, the current trend at different gate voltages and bias voltages was measured on a vacuum probe station when the device did not adsorb and adsorb the target molecules, as shown in fig. 2 (a-d). And the conductance with gate voltage at a bias voltage of 0.1V when the target molecules are not adsorbed and absorbed, as shown in FIG. 2 (e-f). Wherein, the single-layer graphene-silver nanoparticle substrate is soaked in the solution with the concentration of 1x10 -3 The 3-4 hours in the 4NBT of M allows the molecules to be adsorbed uniformly onto the device surface, washed with ethanol after soaking, and dried with high purity nitrogen. FIG. 2 demonstrates the existence of coupling interactions between single-layer graphene and silver nanoparticles, i.e., between surface plasmons and excitons, and directly verifies that the novel devices of the present invention are suitable for electrical measurements;
2) The difference in attenuation intensity (5.36 uW/47.42uW/496.82uW/1.19Mw/2.37mW/4.93 mW) of the 532nm laser (light intensity of about 5 mW) was controlled, and the novel device of the invention was used to determine a Raman spectrum diagram of the molecular reaction kinetics process of the catalytic reaction of 4NBT molecules to DMAB molecules under different light intensities, see FIG. 3, wherein the integration time was 5 seconds, 1109cm -1 And 1306cm -1 Raman characteristic peak belonging to 4NBT, and 1390cm -1 and 1438cm -1 Belongs to the Raman characteristic peak of DMAB. FIG. 4 directly demonstrates that the novel device of the present invention is suitable for laser-modulated surface plasmonsMeasurement of exciton coupling catalytic reaction, and at the same time, surface catalytic reaction can not occur when the laser intensity of 532nm is 5.36uW, so as to provide a control group for the occurrence of photoelectric cooperative regulation catalytic reaction;
3) At 532nm laser intensity of 5.36uW, the bias voltage regulates the occurrence of surface catalytic reaction at 0V/40V, respectively, as shown in FIG. 4 (a-b). Data with a gate voltage of-40V were used as a control group to investigate the electron and hole transfer process in the surface plasmon-exciton coupling effect, see fig. 4 (c). Fig. 4 (d) is a schematic diagram of the electron transfer process in a bias-controlled plasmon-exciton coupling catalytic reaction.
4) At 532nm laser intensity of 5.36uW, the gate voltage regulates the occurrence of surface catalytic reaction at 0V/1V/-1V of the measurement bias, respectively, as shown in FIG. 5 (a-c). Fig. 5 (d) is a schematic diagram of the electron transfer process in a gate voltage modulated plasmon-exciton coupling catalytic reaction.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (4)
1. An optoelectric synergistic surface plasmon-exciton catalytic reaction device characterized by: the semiconductor device comprises a silicon wafer, a two-dimensional semiconductor material (4), a source electrode/drain electrode (2) and incident laser (1), wherein noble metal nano particles are covered on the silicon wafer, the two-dimensional semiconductor material (4) is covered on the noble metal nano particles, the source electrode/drain electrode (2) is positioned on the two-dimensional semiconductor material (4), the silicon wafer is arranged on a base, and gate voltage is introduced to the bottom of the base;
the size and the gap between the two electrodes of the source electrode and the drain electrode (2) can be adjusted, the target molecule (3) is positioned between the two electrodes, and the thickness of the noble metal nano-particles is 1-100nm.
2. The photoelectrocooperating surface plasmon-exciton catalytic reaction device of claim 1 wherein: the silicon wafer comprises SiO 2 Layer (6) and SiA layer (7), wherein the Si layer (7) is covered with SiO 2 And a layer (6).
3. The method for preparing the photoelectric synergistic surface plasmon-exciton catalytic reaction device according to claim 1, characterized in that: the method comprises the following steps:
s1: thermally evaporating noble metal nano particles on a silicon slice of silicon dioxide or monocrystalline silicon to obtain a noble metal nano material substrate;
s2: transferring a two-dimensional semiconductor material onto the noble metal nanoparticle substrate prepared in the step S1, and cleaning to ensure surface cleaning;
s3: evaporating gold/chromium nano particles onto the two-dimensional semiconductor material and metal nano particle composite substrate prepared in the step S2 in a thermal evaporation mode according to the sequence of chromium first and gold later to serve as a source electrode/drain electrode;
s4: the gate voltage is introduced at the bottom of the device fabricated in S3 using the mount.
4. The method for preparing the photoelectric synergistic surface plasmon-exciton catalytic reaction device according to claim 3, which is characterized in that: the thickness of chromium in the S3 is 5nm, and the thickness of gold is 80-100nm.
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| CN105023969A (en) * | 2015-06-11 | 2015-11-04 | 上海电力学院 | A luminous absorption enhanced graphene transistor based on a metal nanostructure |
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