CN120055259A - Silver/transition metal oxyacid salt heterojunction nano material, preparation method and application - Google Patents
Silver/transition metal oxyacid salt heterojunction nano material, preparation method and application Download PDFInfo
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Abstract
本发明涉及复合异质结材料技术领域，公开了一种银/过渡金属氧酸盐异质结纳米材料，所述纳米材料的化学表达式为Ag/AgxMyOz·nH2O，所述纳米材料表面具有银纳米颗粒修饰。该方法包括将银金属电极片置于反应容器的两侧，将过渡金属靶材置于反应容器中央；将高纯去离子水注入反应容器中，并没过靶材表面；在电场诱导下对过渡金属靶材进行液相激光熔蚀反应30min，得到含有所述过渡金属靶材的反应溶液，将含有过渡金属靶材的反应溶液收集在新容器中，并静置两周以上，至反应溶液中出现白色沉淀物，即得Ag/AgxMyOz·nH2O异质结纳米材料。本发明的方法操作简单方便，生产过程中无需添加其他化学试剂，相比水热化学方法更加环保，简便，是首次利用该方法获得该类结构材料。
The invention relates to the technical field of composite heterojunction materials, and discloses a silver/transition metal oxoate heterojunction nanomaterial, wherein the chemical expression of the nanomaterial is Ag/Ag x My O z ·nH 2 O, and the surface of the nanomaterial is modified with silver nanoparticles. The method comprises placing silver metal electrode sheets on both sides of a reaction container, placing a transition metal target material in the center of the reaction container; injecting high-purity deionized water into the reaction container, and not covering the surface of the target material; performing a liquid phase laser ablation reaction on the transition metal target material under electric field induction for 30 minutes to obtain a reaction solution containing the transition metal target material, collecting the reaction solution containing the transition metal target material in a new container, and standing for more than two weeks until a white precipitate appears in the reaction solution, thereby obtaining the Ag/Ag x My O z ·nH 2 O heterojunction nanomaterial. The method of the invention is simple and convenient to operate, and no other chemical reagents need to be added during the production process. Compared with the hydrothermal chemical method, it is more environmentally friendly and simple, and it is the first time that this type of structural material is obtained by using this method.
Description
Technical Field
The invention relates to the technical field of composite heterojunction materials, in particular to a silver/transition metal oxyacid salt heterojunction nano material, a preparation method and application thereof.
Background
The heterojunction is constructed by attaching plasma to a semiconductor material, and the optical and electrical properties of the material can be improved by enhancing mechanisms such as light absorption and scattering, a local electromagnetic field, hot carrier injection, thermal effect and the like through a Local Surface Plasmon Resonance (LSPR) effect. However, at present, the strategy of attaching plasma to a semiconductor nano structure mainly comprises the steps of preparing a semiconductor nano material from various chemical reagents through a wet chemistry method, and then adding the chemical reagent containing noble metal into a suspension of a semiconductor to obtain a noble metal/semiconductor composite structure. However, the hydrothermal reaction generally requires the addition of more chemical reagents, and is more polluted and more complicated in operation steps.
Chinese patent application number 202010108449.5 discloses a nano composite material based on phosphorus-containing molybdenum polyoxometallate, a preparation method thereof, an aptamer sensor and an electrode thereof. The nano composite material comprises carbon, molybdenum disulfide nano sheets and silver-containing nano particles, wherein the nano composite material is obtained by calcining silver-doped phosphomolybdenum polyoxometallate, and the silver-doped phosphomolybdenum polyoxometallate is obtained by reacting silver source, phosphomolybdic acid and thioacetamide. The nano composite material has higher specific surface area and stronger biological affinity, and an electrochemical sensor constructed by the nano composite material has lower detection limit when being used for detecting bisphenol A (BPA), and has high selectivity, good stability and reproducibility, excellent reproducibility and applicability under different environments. However, the method is characterized in that the reaction condition is relatively harsh through hydrothermal reaction and high-temperature calcination. The invention provides a noble metal/transition metal oxyacid salt heterojunction nano material which is convenient to operate, does not need to add chemical reagent and has simple reaction condition, and a novel method. The Ag/Ag xMyOz heterojunction nanostructure is obtained by the method, and is found to be a gas sensor material with good response to hydrogen.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a silver/transition metal oxyacid salt heterojunction nano material, a preparation method and application.
In one aspect, the invention provides a silver/transition metal oxyacid salt heterojunction nanomaterial, wherein the chemical expression of the nanomaterial is Ag/Ag xMyOz·nH2 O, and the surface of the nanomaterial is modified by silver nanoparticles, wherein M is transition metal, x is the number of Ag elements, y is the number of transition metal, z is the number of oxygen elements, and n is the number of water molecules.
Preferably, the diameter of the nano material is 1nm-900nm, and the length is 1 mu m-1000 mu m.
In another aspect, the invention provides a method for preparing a silver/transition metal oxyacid salt heterojunction nanomaterial, comprising the following steps:
Silver metal electrode plates are arranged on two sides of a reaction container, and a transition metal target is arranged in the center of the reaction container;
Injecting deionized water into the reaction vessel and penetrating the surface of the transition metal target;
Carrying out liquid phase laser ablation reaction on the transition metal target under the induction of an electric field to obtain a reaction solution containing the transition metal target;
And collecting the reaction solution containing the transition metal target in a new container, and standing for more than 2 weeks until white precipitate appears in the reaction solution, thus obtaining the Ag/Ag xMyOz heterojunction nano-material.
Preferably, the purity of the silver electrode slice is 99% -99.999%, and the purity of the transition metal target is 99% -99.999%.
Preferably, the deionized water is 2mm-15mm across the surface of the transition metal target.
Preferably, the deionized water has a conductivity of 15mΩ -30mΩ.
Preferably, the laser ablation parameters are 355nm or 532nm wavelength, 1 Hz-10 Hz frequency and 50 mJ-850 mJ/pulse energy.
Preferably, the reaction time is 30min-2h.
Preferably, the electric field has a voltage of 5V-180V.
In still another aspect, the invention also discloses application of the silver/transition metal oxyacid salt heterojunction nano-material gas sensor.
The silver/transition metal oxyacid salt heterojunction nano material, the preparation method and the application thereof have the advantages that the method is simple and convenient to operate, no other chemical reagent is needed to be added in the production process, the method is more environment-friendly and simple and convenient compared with a hydrothermal chemical method, the Ag/Ag xMyOz·nH2 O is synthesized by one step through laser corrosion, the reaction steps are simple, and the structural material is obtained by the method for the first time. The method is a general method, and can replace the target material with other metal target materials to obtain the noble metal/transition metal oxyacid salt heterojunction micro-nano structure material.
Drawings
FIG. 1 is an SEM image of an Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial made in example 1 of the present invention;
FIG. 2 is a TEM image of the Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial and corresponding Ag, mo, O element distribution diagrams prepared in example 1 of the present invention;
FIG. 3 is an XRD pattern of an Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial made in accordance with example 1 of the present invention;
FIG. 4 is a photo-current test chart of the Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial prepared in example 1 of the present invention;
FIG. 5 is a block diagram of a device for preparing Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial according to the present invention.
Detailed Description
As shown in fig. 1-3, the embodiment discloses a silver/transition metal oxyacid salt heterojunction nanomaterial, wherein the chemical expression of the nanomaterial is Ag/Ag xMyOz·nH2 O, and the surface of the nanomaterial is provided with silver nanoparticle modification, wherein M is transition metal, x is the number of Ag, y is the number of transition metal, z is the number of O, and n is the number of H 2 O. The diameter of the nano material is 2nm-900nm, and the length is 2 mu m-1000 mu m.
In the invention, M can represent other transition metal targets such as molybdenum, vanadium, tungsten, niobium, tantalum, titanium and the like, and the obtained nano material can be Ag/AgxMoyOz·nH2O、Ag/AgxVyOz·nH2O、Ag/AgxWyOz·nH2O、Ag/AgxNbyOz·nH2O、Ag/AgxTiyOz·nH2O and the like.
In the invention, a molybdenum target is taken as an example to prepare the Ag/Ag xMoyOz·nH2 O heterojunction nano-material, wherein the values of x, y, z and n slightly differ according to the card library and the laser parameters, and the following examples are shown.
Example 1
As shown in fig. 5, the embodiment provides a preparation method of a silver/transition metal oxyacid salt heterojunction nanomaterial, which comprises the following steps:
S1, placing silver metal electrode plates (purity 99.99%) on two sides of a reaction container, and placing a molybdenum target (purity 99.99%) in the center of the reaction container;
S2, injecting high-purity deionized water (conductivity is 18MΩ) into a reaction vessel, and enabling the deionized water to be 2mm beyond the surface of the molybdenum target;
s3, turning on a laser, a direct-current reaction power supply, and carrying out liquid-phase laser ablation reaction on a molybdenum target for 30min under the induction of an electric field (voltage is 5V) to obtain a reaction solution containing the molybdenum target, wherein the laser ablation parameters are that the wavelength is 532nm, the frequency is 10Hz, and the energy is 600mJ/pulse;
And S4, collecting a reaction solution containing the molybdenum target in a new container, and standing for 2 weeks until white precipitate appears in the reaction solution, thus obtaining the Ag/Ag 2Mo3O10·1.8H2 O heterojunction nano-material. The whole synthesis method does not need to add other chemical reagents or multi-step reaction, and is more convenient and environment-friendly compared with the existing method.
Fig. 1 shows SEM morphology of Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial in this example. In fig. 1, the left graph shows a low-power SEM morphology graph of the Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial, the right graph shows a high-power graph, the Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial is fibrous, dislocation networks are formed by high-density dislocations, and the surface of the nanomaterial is modified by Ag particle materials.
Fibrous nanomaterials have extremely high specific surface areas, which means that they are able to provide more gas adsorption sites. When gas molecules adsorb on the surface of a material, they physically or chemically interact with the material, thereby changing the electrical properties (e.g., resistance or capacitance) of the material. The high specific surface area enables the fibrous nanomaterial to more effectively adsorb target gas molecules, thereby improving the sensitivity of the sensor.
Fibrous nanomaterials generally have good electrical properties such as high electrical conductivity and low electrical resistance. This enables them to respond quickly to electrical changes in the gas adsorption and desorption processes, thereby enabling quick detection. The surface chemistry of the fibrous nanomaterials can be controlled by a variety of methods, such as doping, surface modification, or compounding with other materials. These methods can change the selectivity of the material for a particular gas, thereby improving the detection accuracy of the sensor. Silver nano particles are decorated on the surface of the metal oxide nano fiber, so that the detection performance of the silver nano particles on gas can be remarkably improved.
In conclusion, the fibrous nano material prepared by the embodiment has important application value in the gas sensor due to the unique physical and chemical properties, can remarkably improve the sensitivity, selectivity and stability of the sensor, and simultaneously reduces the working temperature and energy consumption.
Fig. 2 shows a TEM image of an Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial and corresponding elemental profiles of Ag, mo, O in this example. The graph (1) is a TEM morphology graph of a single Ag/Ag 2Mo3O10·1.8H2 O heterojunction nano-material, the graph shows that the surface of the nano-material is modified by a plurality of granular materials, and the right three graphs of the graph (1) are corresponding Ag, mo and O element distribution graphs, so that the long nano-wire is provided with Ag, mo and O elements, granular substances only contain Ag elements, do not contain O elements and are silver nano-particles. Thus, a Ag 2Mo3O10·1.8H2 O nanostructure was obtained with a structure modified by Ag particles.
Fig. 3 shows the XRD patterns of the Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial in this example, and it can be seen from the figure that the XRD patterns have 7 peaks, and the remaining 6 diffraction peaks are respectively at 11.25 ̊, 13.40 ̊, 28.26 ̊, 35.15 ̊, 38.07 ̊, 46.26 ̊, and respectively correspond to (101), (200), (103), (501), (230), and (404) crystal planes of Ag 2Mo3O10·1.8H2 O (JCPDS No. 39-0045), except that the peak with the highest diffraction intensity is the peak of the silicon substrate.
Example 2
The embodiment provides a preparation method of a silver/transition metal oxyacid salt heterojunction nano material, which comprises the following steps:
silver metal electrode pieces (purity 99.9%) are placed on two sides of a reaction vessel, and a molybdenum target (purity 99.9%) is placed in the center of the reaction vessel;
injecting high-purity deionized water (conductivity is 15MΩ) into the reaction vessel, and soaking the surface of the molybdenum target for 5mm;
Turning on a laser, a direct-current reaction power supply, and carrying out liquid phase laser ablation reaction on a molybdenum target for 50min under the induction of an electric field (voltage is 150V) to obtain a reaction solution containing the molybdenum target, wherein the laser ablation parameters are 355nm in wavelength, 1Hz in frequency and 50mJ/pulse in energy;
And collecting the reaction solution containing the molybdenum target in a new container, and standing for 3 weeks until white precipitate appears in the reaction solution, thus obtaining the Ag/Ag 2Mo5O14·2H2 O heterojunction nano-material.
Example 3
The embodiment provides a preparation method of a silver/transition metal oxyacid salt heterojunction nano material, which comprises the following steps:
silver metal electrode pieces (purity 99.0%) are placed on two sides of a reaction vessel, and a molybdenum target (purity 99.0%) is placed in the center of the reaction vessel;
injecting high-purity deionized water (conductivity: 18mΩ) into the reaction vessel, and passing 10mm beyond the surface of the molybdenum target;
Turning on a laser, a direct-current reaction power supply, and carrying out liquid phase laser ablation reaction on a molybdenum target for 1h under the induction of an electric field (voltage is 50V) to obtain a reaction solution containing the molybdenum target, wherein the laser ablation parameters are 355nm in wavelength, 5Hz in frequency and 300mJ/pulse in energy;
and collecting the reaction solution containing the molybdenum target in a new container, and standing for 4 weeks until white precipitate appears in the reaction solution, thus obtaining the Ag/Ag 3Mo6O18·5H2 O heterojunction nano-material.
Example 4
The embodiment provides a preparation method of a silver/transition metal oxyacid salt heterojunction nano material, which comprises the following steps:
silver metal electrode pieces (purity 99.9%) are placed on two sides of a reaction vessel, and a molybdenum target (purity 99.9%) is placed in the center of the reaction vessel;
Injecting high-purity deionized water (conductivity: 18mΩ) into the reaction vessel, and passing 8mm beyond the surface of the molybdenum target;
Turning on a laser, a direct-current reaction power supply, and carrying out liquid phase laser ablation reaction on a molybdenum target for 1h under the induction of an electric field (voltage is 50V) to obtain a reaction solution containing the molybdenum target, wherein the laser ablation parameters are that the wavelength is 532nm, the frequency is 6Hz, and the energy is 350mJ/pulse;
And collecting the reaction solution containing the molybdenum target in a new container, and standing for 4 weeks until white precipitate appears in the reaction solution, thus obtaining the Ag/Ag 3Mo5O16·3H2 O heterojunction nano-material.
Example 5
The embodiment provides a preparation method of a silver/transition metal oxyacid salt heterojunction nano material, which comprises the following steps:
Silver metal electrode plates (purity 99.99%) are arranged on two sides of a reaction container, and a molybdenum target (purity 99.99%) is arranged in the center of the reaction container;
injecting high-purity deionized water (with the conductivity of 30MΩ) into the reaction vessel, and soaking the surface of the molybdenum target for 12mm;
Turning on a laser, a direct-current reaction power supply, and carrying out liquid phase laser ablation reaction on a molybdenum target for 1.5h under the induction of an electric field (voltage is 100V) to obtain a reaction solution containing the molybdenum target, wherein the laser ablation parameters are that the wavelength is 532nm, the frequency is 3Hz, and the energy is 400mJ/pulse;
And collecting the reaction solution containing the molybdenum target in a new container, and standing for 5 weeks until white precipitate appears in the reaction solution, thus obtaining the Ag/Ag 3Mo3O12·4H2 O heterojunction nano-material.
Example 6
The embodiment provides a preparation method of a silver/transition metal oxyacid salt heterojunction nano material, which comprises the following steps:
silver metal electrode plates (purity 99.999%) are arranged on two sides of a reaction container, and a molybdenum target (purity 99.999%) is arranged in the center of the reaction container;
Injecting high-purity deionized water (conductivity 20MΩ) into the reaction vessel, and soaking the surface of the molybdenum target for 15mm;
Turning on a laser, a direct-current reaction power supply, and carrying out liquid phase laser ablation reaction on a molybdenum target for 2 hours under the induction of an electric field (voltage of 180V) to obtain a reaction solution containing the molybdenum target, wherein the laser ablation parameters are that the wavelength is 532nm, the frequency is 8Hz, and the energy is 850mJ/pulse;
And collecting the reaction solution containing the molybdenum target in a new container, and standing for 6 weeks until white precipitate appears in the reaction solution, thus obtaining the Ag/Ag 4Mo5O18·3H2 O heterojunction nano-material.
Application example 1
The Ag/Ag 2Mo3O10·1.8H2 O heterojunction nanomaterial prepared in example 1 is applied to a gas sensor.
The Ag/Ag 2Mo3O10·1.8H2 O heterojunction is made into a gas sensor, and the sensor is connected with an external circuit to capture the signal change of current or resistance. Its current response was tested in different hydrogen concentration environments to obtain the data of fig. 4. Experiments show that the Ag/Ag 2Mo3O10·1.8H2 O heterojunction has obvious current signal response to hydrogen. The detection limit of the gas sensor for hydrogen at 350 ℃ is 10ppm.
In the description of the present invention, it should be understood that the azimuth or positional relationships indicated by the azimuth words such as "front, rear, upper, lower, left, right", "lateral, vertical, horizontal", and "top, bottom", etc., are generally based on the azimuth or positional relationships shown in the drawings, merely to facilitate description of the present invention and simplify the description, and these azimuth words do not indicate or imply that the apparatus or elements referred to must have a specific azimuth or be constructed and operated in a specific azimuth, and thus should not be construed as limiting the scope of protection of the present invention.
It will be apparent to those skilled in the art from this disclosure that various other changes and modifications can be made which are within the scope of the invention as defined in the appended claims.
Claims (10)
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