KR101645661B1 - Hydrogen sensor based on platinum/palladium-graphene hybrid and method of fabricating the same - Google Patents
Hydrogen sensor based on platinum/palladium-graphene hybrid and method of fabricating the same Download PDFInfo
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- KR101645661B1 KR101645661B1 KR1020140183437A KR20140183437A KR101645661B1 KR 101645661 B1 KR101645661 B1 KR 101645661B1 KR 1020140183437 A KR1020140183437 A KR 1020140183437A KR 20140183437 A KR20140183437 A KR 20140183437A KR 101645661 B1 KR101645661 B1 KR 101645661B1
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Abstract
The present invention relates to a platinum / palladium core-cell graphene hybrid-based hydrogen sensor and a method of manufacturing the same, wherein the graphene supported on a Pt / Pd (platinum / palladium) core- . The Pt / Pd core - cell was synthesized by a two - step chemical route (seed - mediated growth) and a polymer assisted growth process. A very uniform colloidal palladium (Pd) nanocube at 30 nm in size was used as the core and a thin layer of platinum (Pt) was coated on the outer surface of each Pd core as a cell; The Pt / Pd core-cell was simply decorated with graphene flake by hydrazine in an easy first step reaction. The results for the Pt / Pd core-cell-graphene hybrid have been applied as a new hydrogen detection material due to its broad detection range, high sensitivity and fast reaction / recovery time advantages. Resistive sensors using the Pt / Pd core-cell-graphene hybrid have a detection range of 40,000 to 1 ppm with reliable reliability at room temperature. The hydrogen sensor had a large reaction value of 36% and a reaction / recovery time of 3 / 1.2 minutes at 1% hydrogen concentration at room temperature.
Description
The present invention relates to a platinum / palladium core-cell graphene hybrid-based hydrogen sensor and a method of manufacturing the same. More particularly, the present invention relates to a platinum- / Pd core-cell were synthesized and attached to a large amount of graphene (Gr) flakes to synthesize Pt / Pd core-cell-Gr hybrids. Platinum prepared by using this Pt / Pd core- / Palladium core-cellgaphene hybrid-based hydrogen sensor and a method of manufacturing the same.
Graphene oxide (GO) and reduced graphene oxide (RGO) are widely used for a variety of applications including energy, photocatalysis, biotechnology, medical and sensing. Despite the interest of research groups in gas sensing, the sensitivity of graphene-based sensors for specific gas / biomolecule targets can be measured using hybrid structures, or nanomaterials, in combination with nanomaterials, Demand. Graphene obtained from the reduction of GO using a reducing agent showed weak gas molecular sensitivity due to addition of other nitrogen functional groups leading to unstable RGO. However, functionalized graphene through noble metal catalysts not only improves sensitivity and selectivity towards target gases, but also exhibits sensor stability in humid environments.
Hydrogen (H 2 ) sensors are indispensable for safety and are widely needed for a variety of applications. Current demands for hydrogen sensors include high sensitivity and fast reaction times at low operating temperatures to raise the level to a small ppm. Hydrogen sensors functioning at room temperature are desirable to address the power consumption given to the sensor chip, which is caused by supply heat and ignition exposure at high hydrogen (H 2 ) concentrations. Sensors based on nanomaterials offer a potential solution due to their high surface to volume ratio. Nanomaterials based on conventional hydrogen sensors include polymers, metal oxide nanostructures, and carbon-based materials (carbon nanotubes and graphene). Among these options, carbon-based hydrogen sensors maintain distinct advantages in the areas of sensitivity, stability, the ability to steer harsh environments, and the ability to function in a liquid environment, as well as the ability to function in an oxygen-free environment. In addition, noble metal catalysts containing platinum (Pt), palladium (Pd), gold (Au), silver (Ag), titanium (Ti), and nickel (Ni) Material is added. Due to this low hydrogen dissociation action, Au, Ag, Ti and Ni do not provide optimal function. Among these metal catalysts, Pt and Pd are most efficient at hydrogen (H 2 ) dissociating to H + protons at room temperature. Recently, two metal catalysts have been used to enhance the performance of catalysts with advantages in terms of catalyst control, morphology and synergy.
In the inventor's previous invention, catalysts based on Pt and Pd have been extensively discussed in the ongoing development of hydrogen sensors with significant issues of high sensitivity at room temperature. So far, Pt and Pd based catalysts have been used primarily as efficient catalysts in resistive based hydrogen sensors. Despite the great advantages of Pt-based catalysts in hydrogen sensing, many costly problems remain in Pt materials. The core-shell structure is a great way to reduce the Pt loading catalyst. Therefore, the Pt-cell case was discussed to enable efficient cost design. In addition, both Pt and Pd catalysts exhibit very good hydrogen catalytic activity and sensitivity. A good Pt-Pd core-cell for hydrogen detection is due to the nature of the interactions between the core and the cell and their contact points, the high surface-to-volume ratio as well as the quantum size in the core-cell form of the two functions. Moreover, Pd NPs (palladium nanoparticles) will expand its volume during hydrogen adsorption / desorption and will cause hysteresis behavior in a resistive hydrogen sensor as discussed in our previous invention. By coating the Pt cell on the outer surface of the Pd nanocube, the Pt cell will compress the Pd extension and lead to reducing the hysteresis in the sensor. In addition, Pt cell growth on the Pd core will greatly impose huge defects at the interface of the core-cell boundary of the Pt / Pd nanoparticles, playing the most important role in enhancing the sensitivity of the hydrogen sensor.
Various nanocrystalline Pd have high catalytic activity and are reported to be a good starting material for building a hybrid or core-cell structure. The demand for hydrogen sensors based on Pd provides a challenge to develop new efficient catalysts for hydrogen detection as well as for hydrogen storage. However, the application of these pure Pd nanocrystalline catalysts for hydrogen detection is uncommon to be achieved due to the loss of the connection between the complex manufacturing process and the Pd nanocrystals. Graphene (Gr), a two-dimensional material, exhibits excellent electrical and mechanical properties and is well known as a potential material for supporting metal catalysts or forming metal graphene composites / hybrids. In the previous invention of the present inventor, we prepared a Pd-Gr graphene complex / hybrid, wherein Pd changed shape from nanoparticles to nanocubes and then applied as a resistance-based hydrogen sensor. From our previous experiments, the Pd-Gr graphene complex / hybrid shows the potential for hydrogen detection at low temperatures. However, the detection range of the hydrogen concentration was limited to 0.2 to 10,000 ppm from the present invention of the present inventor.
SUMMARY OF THE INVENTION The present invention has been made in order to overcome the above problems, and it is an object of the present invention to disclose the largest hydrogen detection range and to develop a new efficient catalyst for hydrogen detection. The Pt / Pd core- The Pt / Pd core-shell structure can be obtained by applying Pt as a core to a Pd nanocube as a core by a chemical method through seed mediated growth and applying it as a catalyst for detecting hydrogen gas by attaching it to a graphene flake in a large amount, The present invention provides a platinum / palladium core-cell graphene hybrid-based hydrogen sensor and a method of manufacturing the same, wherein the cell graphene hybrid is used as an excellent catalyst material for hydrogen detection.
In order to achieve the above object, the platinum / palladium core-cell graphene hybrid-based hydrogen sensor of the present invention comprises platinum (Pt) used as a cell on the outer surface of a palladium (Pd) nanocube used as a core, Using the layer coated Pd / Pt core-cell as a catalyst for hydrogen detection, the Pd / Pt core-cell was dispersed in a graphene flake formed from a graphene oxide (GO) by a reducing agent, And the Pd / Pt core-cell of the Pd / Pt core-cell is attached to the graphene flake.
The palladium (Pd) nanocube is preferably a colloidal nanocube having a size of 30 to 40 nm.
The hydrogen (H 2 ) detection range of the hydrogen sensor is preferably 1 to 40,000 ppm.
In the method for producing a platinum / palladium core-cell graphene hybrid-based hydrogen sensor according to the present invention, a palladium (Pd) nanocube solution is synthesized using a potassium chlorate palladium (K 2 PdCl 4 ) solution at a predetermined concentration; The palladium nanocube solution mixed by the above step is mixed with a certain concentration of chloroplatinic acid hexaphosphate (H 2 PtCl 6 .6H 2 O), CTAB, PVP (poly-vinylpyrrolidone) and ascorbic acid to prepare a mixture Synthesizing; Centrifuging and washing the mixture and re-diffusing it with deionized water to form a Pd / Pt core-cell aqueous solution; Adding the Pd / Pt core-cell aqueous solution to a graphene oxide (GO) aqueous solution together with a reducing agent to synthesize a Pd / Pt core-cellgaphene hybrid mixture; Coating said mixture on a SiO 2 / Si base on a hot plate by spraying as a suspension; Depositing a noble metal on the surface of the Pt / Pd-Gr / SiO 2 / Si base formed by coating the mixture to form an ohmic contact layer; And annealing the Pt / Pd-Gr / SiO 2 / Si sensor chip formed by forming the ohmic contact layer by post-annealing.
The reducing agent is preferably a reducing agent hydrate (N 2 H 4 .H 2 O) of 65 wt%.
Further it is preferred to heat the SiO 2 / Si base on the hot plate at a constant temperature when spraying the nano-composite mixture on the SiO 2 / Si base.
The ohmic contact layer is preferably formed by a metal mask and RF sputtering.
The post-annealing is preferably performed in an argon (Ar) gas atmosphere at 400 ° C for 30 minutes.
According to the platinum / palladium core-cell graphene hybrid-based hydrogen sensor of the present invention and the method of manufacturing the same, platinum used as a cell for the palladium nanocube used as a core is coated with a thin layer, It has a wide detection range of hydrogen and a large reaction value, and shows rapid reaction / recovery time at room temperature, which leads to reliable stability and reliability of the hydrogen sensor.
FIG. 1 is a SEM image showing (a) Pd nanocube as a seed and (b) Pt-Pd core-cell
Figure 2 is a TEM image showing (a) pure Pt-Pd core-cell and (b) Pt-Pd core-cell-graphene hybrid
FIG. 3 illustrates the relationship between (a) EDS color mapping and EDS scanning lines at different positions in
Figure 4 (a) shows the hydrogen of Pt-Pd core-cell-Gr hybrids at different hydrogen concentrations that are tested in real time for reproducibility in 4 cycles of 4% hydrogen and hysteresis properties (at 3% and 1% (B) is a linear correction graph by the Langmuir model,
FIG. 5 is a graph showing the response of a hydrogen sensor in a range of (a) high and (b) low hydrogen concentration
Hereinafter, preferred embodiments of a platinum / palladium core-cell graphene hybrid-based hydrogen sensor and a method of manufacturing the same according to the present invention will be described in detail with reference to the accompanying drawings. It is to be understood that the present invention is not limited to the disclosed embodiments, but may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, It is provided to inform.
A method of manufacturing a platinum / palladium core-cellgraffin hybrid-based hydrogen sensor according to the present invention will be described in detail as follows.
First, the production of the hydrogen sensor according to the present invention will be described through an experimental procedure as follows.
1. Experiment
1.1 Pt / Pd Synthesis of core-cell solution
The Pd nanocube seed solution was synthesized from the previous invention very uniformly in a size of 30 nm. That is, a solution of potassium tetrachloride palladium (K 2 PdCl 4 ) in a predetermined concentration is added to cetyltrimethylammonium bromide (CTAB), stirred, and ascorbic acid solution is added to the solution at a time lag. (K 2 PdCl 4 ), cetyltrimethylammonium bromide (CTAB) and ascorbic acid solution were mixed and stirred in the prepared seed solution to prepare palladium (Pd) nanocube solution .
On the Pd cube as the seed, the Pt cells were combined with 2 ml of an aqueous solution of 5 mM H 2 PtCl 6 .6H 2 O (chlorplatinic acid hexahydrate, Sigma-Aldrich) and 1.5 ml of the Pd nanocubide suspension as described above in 50 ml Of an aqueous solution of 100 mM cetyltrimethylammonium bromide (CTAB). Subsequently, 6 ml of PVP (poly-vinylpyrrolidone, Sigma-Aldrich) was added followed by the addition of 700 μl of freshly prepared 250 mM ascorbic acid, Lt; / RTI > Finally, the resulting black solution of the Pt / Pd core-cell was centrifuged at 1000 rpm for 30 minutes and washed for 5 hours to remove excess surfactant and reducing agent. Finally, the black product isolated was resuspended in 5 mL DI water.
1.2 Pt / Pd The core-cell- Grapina Hybrid synthesis
Graphen oxide (GO) was prepared from extra pure graphite powder (Merck, 99.99%) according to the Hummers method. The GO suspension of GO (10 mg / ml) was diluted with 2N, N-dimethylformamide (DMF, Sigma-Aldrich) at a concentration of 2 mg / ml and homogenized in DMF / water (80:20 v / v) And sonicated in an ultrasonic bath for 1 hour to generate one suspension. At this time, 5 ml of the Pt / Pd core-cell was added to this aqueous solution with stirring. Then 1 ml of hydrazine monohydrate (N 2 H 4 .H 2 O, Sigma-Aldrich, 65% by weight) was added to the mixture with a reducing agent with further stirring at an elevated temperature of 80 ° C for 6 hours. The resulting suspension was black in color and used to fabricate a resistive hydrogen sensor. The basic manufacturing steps are as follows: The Pt / Pd core-cell-Gr hybrid was coated onto an SiO 2 / Si base via airbrush spray (Hansa 381, N 2 as carrier gas) with 5 ml of the suspension. The SiO 2 / Si base sensor chip was divided into several pieces with a fixed size of 0.5 × 1
After the above steps, the annealing process was applied to improve the safety of Pt / Pd graphene bonding for hydrogen sensing in all samples as well as Pt / Pd. This was accomplished by using Nextron RTP-1200 in an argon (Ar) gas atmosphere at 400 < 0 > C for 30 minutes to complete the production of the hydrogen sensor.
The surface of the Pt / Pd core-cell-Gr hybrid was characterized using a JSM-6500F Field Emission Scanning Electron Microscope (FE-SEM). Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) images of Pt / Pd core-cell-Gr hybrids were displayed using an ultra-high resolution radiation electron microscope (JEOL JEM-2100F). Component analysis by EDS (Energy Dispersive X-ray Spectrometer) mapping and EDS (Energy Dispersive X-ray Spectrometer) scanning line was performed by TEM equipment (JEOL JEM-2100F). The sensor was installed inside a chamber of enclosed environment, and the Keithley probe station (SCS-4200) with the bias voltage fixed at 1V recorded the resistance value of the sensor. A computerized mass flow controller (ATOVAC, GMC 1200) system was used to change the concentration of hydrogen in synthetic air (Deokyang Co., Ltd.). The gas mixture was delivered at a constant flow rate of 50 standard cubic centimeters per minute (sccm) with different hydrogen concentrations. The gas chamber was cleaned with synthetic air between each hydrogen pulse to allow the surface of the sensor to return to atmospheric conditions.
2. Results and discussion
Figure 1 (a) shows a successful synthesis of Pd nanocube seeds by a two-step chemical route. Pd nanocubes as seeds are very uniform and well distinguishable in size (30-40 nm). Pd nanocubes were prepared from an aqueous solution of potassium pantalate (II) palladium (K 2 PdCl 4 ) together with ascorbic acid as a reducing agent in the presence of CTAB as a stabilizer. The synthesis of metal nanoparticles with controlled size and shape depends on the variety of reducing parameters, such as solvent and temperature, as well as metal precursors, surfactants / stabilizers, reducing agents, and impurity ions. In this case, in the presence of CTAB as a stabilizer, the reduced metal ion PdCl 4 2 - by ascorbic acid resulted in rapid Pd nucleation following the (100) - plane direction. Pd nanocubes were characterized by Pd nanoparticles (111) - plane of the (old). The size of the Pd nanocubes can be controlled by varying the concentration of the Pd precursor, the amount of the Pd seed solution, the temperature, and the reaction time. In this case, the smallest size of Pd nanocubes of 30-40 nm was used as the Pd seed layer (as the core). The choice of the smallest Pd nanocube as the core would yield a small Pt-Pd core-cell structure, which increased the volume-to-total surface area ratio in the Pt-Pd core-cell-Gr hybrids. FIG. 1 (b) shows the success of the Pt / Pd core-cell, which includes a Pd cube as a core and a thin layer of Pt as a cell, grown by a seed-mediated process in two steps. The Pt / Pd core-cell has a size of approximately 50-60 nm with the first 30 minute growth. In Figure 1 (b), two distinct colors in each nanoparticle represent the core-cell structure. Because of the electron transport of the Pt material, the Pd cores can be observed even when they are hidden inside the Pt cell layer. Pt conducts the electron beam through itself and the interface with the surface inside the Pd nanocube, and the resultant on the Pt / Pd core-cell can be clearly seen by the SEM equipment.
Figure 2 shows a TEM analysis of a pure Pt / Pd core-cell and a Pt / Pd core-cell decorated with graphene. Figure 2 (a) shows the high resolution of single Pt-Pd core-cell nanoparticles. The Pt / Pd core-cell became thick nanoparticles (NPs) after 2 hours of reaction. As a cell layer, Pt grew on the Pd cube in a highly porous state as shown in Fig. 2 (a). The natural lattice mismatch between the two different materials caused this porosity in the Pt cell layer. In Fig. 2 (a), the Pt cell layer was composed of many cylinders on the Pd cube surface. Graphene was transparent and well dispersed in Pt / Pd core-cell nanoparticles. In the synthesis of Pt / Pd core-cell-graphene hybrids, hydrazine as a common reducing agent of graphene oxide (GO) will remove the oxygen functional groups attached to the graphene oxide (GO) Cell nanoparticles. The resulting graphene surrounded by the Pt / Pd core-cell formed a hybrid with many distinct Pt / Pd core-cells attached to the graphene flakes, as shown in Figure 2 (b). Extremely thin graphene flakes with good mechanical properties can include Pt / Pd core-cells during hybrid synthesis and extra processing required for sensor fabrication. However, from FIGS. 1 and 2, the Pt / Pd core-cell in the present invention is not uniform in size and shape, but needs to be improved in the future.
The EDS mapping in FIG. 3 confirmed the success of the Pt / Pd core-cell at two different locations. In green, Pd was located inside the blue color indicating the Pt component. The EDS line scan from the TEM instrument shows Pt as a cell and Pd as a core in Pt / Pd nanoparticles. EDS line scan showed non-uniformity of the nanoparticle surface. At the center of the core-cell nanoparticles, the strength of the Pt component was decreased particularly by increasing the strength of the Pd component in Fig. 3 (b). The EDS analysis in FIG. 3 confirms this by SEM and TEM analysis in FIGS. 1 and 2 where the unevenness of the Pt / Pd core-cell structure needs to be improved in the future.
Figure 4 (a) shows the reaction of a resistive hydrogen sensor based on Pt / Pd core-cell-Gr hybrids at various hydrogen concentrations at room temperature. In general, the sensor will have a clear response between 1 and 40,000 ppm hydrogen and a different hydrogen gas concentration (from 4% to 6 ppm), with increased reproducibility between increased resistance after exposure to hydrogen gas and hydrogen per cycle (4% hydrogen) Respectively. The sensor response value S was defined as the ratio of the resistance change of the resistive sensor at a bias voltage (1 V) fixed by exposure to hydrogen gas as in the following equation:
Where R a is the resistance of the sensor in the presence of synthetic air alone and R g is the resistance in the presence of hydrogen at a constant concentration.
Reaction value S reached 50% with a hydrogen concentration of 4%. In particular, a hydrogen sensor based on a Pt / Pd core-cell can utilize a hydrogen detection range from 6 to 40,000 ppm as in Figure 4 (a). Therefore, the discovery of the synergistic effect has been intensively studied. The result is an enhanced catalytic activity of the Pt / Pd core-cell. At present, hydrogen molecule adsorption plays a most important role in enhancing the hydrogen sensing property at the interface of the core-cell interface of Pt / Pd nanoparticles. This also provides an engineering opportunity for highly efficient functional materials for hydrogen storage using two metal Pt / Pd. With a certain hydrogen separation nature, the Pt cell constantly leads to hydrogen passage and interacts with Pd in the core. By this mechanism, the hydrogen sensor showed a wide detection range and high sensitivity. Hydrogen adsorption in Pd materials such as thin films, nanodiscs and nanowires showed destruction to the Pd structure after several hydrogen adsorption cycles. However, in the present invention, the Pt / Pd core-cell still works well after 4 cycles with a high concentration of hydrogen (4%). No spikes were observed in the reaction signal for several hours during testing of these hydrogen sensors based on Pt / Pd core-cells. Furthermore, the hysteresis phenomenon was tested in Figure 4 (a). The reaction value of the hydrogen sensor after 4 cycles with 1% and 3% and 4% high hydrogen concentration is the same as in FIG. 4 (b), showing a certain stability of Pt / Pd core-cell during hydrogen adsorption / desorption , The Pt cell compresses the fracture to the Pd structure while interacting with the hydrogen molecule.
The linear relationship between the sensitivity and the square root of hydrogen is believed to be due to the Langmuir isotherm theory of gas sorption. It is suggested that hydrogen adsorption, which is proportional to the coverage ratio (?) Of hydrogen on the surface and linearly affects the effective charge concentration in the sensing film, such as the Sun, changes the Pd action function. Therefore, the resistance change, ΔR / R air, is proportional to θ. The proposed reaction for hydrogen separation on the Pd surface is as follows:
The linear relationship between the sensitivity and the square root of hydrogen is believed to be due to the Langmuir isotherm theory of gas sorption. It is suggested that hydrogen adsorption, which is proportional to the coverage ratio (?) Of hydrogen on the surface and linearly affects the effective charge concentration in the sensing film, such as the Sun, changes the Pd action function. Therefore, the resistance change, ΔR / R air, is proportional to θ. The proposed reaction for hydrogen separation on the Pd surface is as follows:
Where S Pd was proposed to be able to use the Pd surface site and to be proportional to the total [theta]. According to the Langmuir isotherm at equilibrium, the desorption rate is equal to the adsorption rate as shown in the following equation (2) or (3).
Where k a and k b are the adsorption and desorption constants and P is the hydrogen partial pressure. Using the above equation (3), the resistance change at a low coverage (? <1) of hydrogen is given by the following equation (4)
Where θ is the hydrogen shear,? Is the resistance change in the hydrogen adsorption, R air is the fundamental resistance, and K is the equilibrium constant. Therefore, the sensor response value S shows a linear correction to the square root of the hydrogen concentration as shown in Fig. 4 (b). Figures 5 (a) and 5 (b) confirm that hydrogen sensors based on Pt / Pd core-cells are available for both high and low hydrogen concentration ranges, as in Figures 5 (a) and 5 (b). The hydrogen sensor showed a definite linearity in the hydrogen concentration range of 6 to 40,000 ppm, and the detection limit (LOD) was 1 ppm as in FIG. 5 (b) due to the reliable conductivity and low noise level nature of the graphene material.
3. Conclusion
In the present invention, the inventors synthesized Pt / Pd core-cell-Gr hybrids for application to hydrogen detection through simple chemical methods. The Pt / Pd core-cell used as the hydrogen catalyst is approximately 100 nm in size and is well dispersed with graphene flakes. Compared to our previous invention in Pd-Gr composites / hybrids for hydrogen sensors, the Pt / Pd core-cell hybrids have about four times higher sensitivity. The reaction value with 10,000 ppm hydrogen is 36% at room temperature. Hydrogen sensors based on Pt / Pd core-cell-Gr hybrids have an apparent linear response with hydrogen from 40,000 to 1 ppm even at room temperature. The response / recovery time of the hydrogen sensor is very fast, with 1% hydrogen at 3 / 1.2 min. From the inventor's experiments, hydrogen sensors based on Pt / Pd core-cell-Gr hybrids work well at large and low hydrogen concentrations, even at low temperatures, and are promising as new hydrogen storage materials as well.
As described above, the platinum / palladium core-cell graphene hybrid based hydrogen sensor according to the present invention and the method of manufacturing the same are described with reference to the drawings. However, the present invention is limited by the embodiments and the drawings disclosed herein It is needless to say that various modifications can be made by those skilled in the art within the scope of the technical idea of the present invention.
Claims (8)
Wherein the palladium (Pd) nanocube is a colloidal nanocube having a size of 30 to 40 nm.
Wherein the hydrogen sensor (H 2 ) detection range of the hydrogen sensor is 1 to 40,000 ppm.
Synthesizing a palladium (Pd) nanocube solution using a solution of potassium tetrachloride palladium (K 2 PdCl 4 ) at a predetermined concentration;
The palladium nanocube solution mixed by the above step is mixed with a certain concentration of chloroplatinic acid hexaphosphate (H 2 PtCl 6 .6H 2 O), CTAB, PVP (poly-vinylpyrrolidone) and ascorbic acid to prepare a mixture Synthesizing;
Centrifuging and washing the mixture and re-diffusing it with deionized water to form a Pd / Pt core-cell aqueous solution;
Adding the Pd / Pt core-cell aqueous solution to a graphene oxide (GO) aqueous solution together with a reducing agent to synthesize a Pd / Pt core-cellgaphene hybrid mixture;
Coating said mixture on a SiO 2 / Si base on a hot plate by spraying as a suspension;
Depositing a noble metal on the surface of the Pt / Pd-Gr / SiO 2 / Si base formed by coating the mixture to form an ohmic contact layer; And
Wherein the Pt / Pd-Gr / SiO 2 / Si sensor chip is formed by forming the ohmic contact layer on the Pt / Pd-Gr / SiO 2 / Si sensor chip. Gt;
Wherein the reducing agent is a reducing agent hydrate (N 2 H 4 .H 2 O) in an amount of 65 wt%.
Wherein the SiO 2 / Si base on the heating plate is heated to a predetermined temperature when the nanocomposite mixture is sprayed onto the SiO 2 / Si base.
Wherein the Ohmic contact layer is formed by RF sputtering with a metal mask. ≪ RTI ID = 0.0 > 15. < / RTI >
Wherein the heat treatment of the post-annealing is performed in an argon (Ar) gas atmosphere at 400 ° C for 30 minutes.
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| CN109709188B (en) * | 2019-02-27 | 2020-08-11 | 山东理工大学 | Preparation method and application of sandwich type immunosensor marked by nitrogen-sulfur double-doped graphene oxide |
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