CN114195146A - Preparation method and application of composite material of expanded graphite in-situ grown silver nanoparticles - Google Patents
Preparation method and application of composite material of expanded graphite in-situ grown silver nanoparticles Download PDFInfo
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- CN114195146A CN114195146A CN202111381652.0A CN202111381652A CN114195146A CN 114195146 A CN114195146 A CN 114195146A CN 202111381652 A CN202111381652 A CN 202111381652A CN 114195146 A CN114195146 A CN 114195146A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 69
- 239000010439 graphite Substances 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 28
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052709 silver Inorganic materials 0.000 claims abstract description 19
- 239000004332 silver Substances 0.000 claims abstract description 19
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims abstract description 14
- 229940071536 silver acetate Drugs 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 claims abstract description 12
- 238000001514 detection method Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 238000001069 Raman spectroscopy Methods 0.000 claims description 12
- 239000004570 mortar (masonry) Substances 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 230000005284 excitation Effects 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000758 substrate Substances 0.000 abstract description 5
- 230000005672 electromagnetic field Effects 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract 2
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 7
- 238000001354 calcination Methods 0.000 description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 238000000479 surface-enhanced Raman spectrum Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000011835 investigation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method and application of a composite material of expanded graphite in-situ grown silver nanoparticles. The high-temperature calcination method is adopted, and comprises the steps of utilizing the mixture of the expanded graphite and the silver acetate to decompose the silver acetate at high temperature in an inert atmosphere, and generating a silver simple substance on the surface of the expanded graphite in situ. The size and density of silver particles on the surface of the expanded graphite can be regulated and controlled by regulating the molar mass ratio of the silver acetate to the expanded graphite. The composite material not only has good adsorbability, but also has a plasmon electromagnetic field enhancement effect, and if the composite material is used as a substrate, the surface enhanced Raman spectroscopy detection of various trace substances can be realized. The preparation method of the material does not need a surfactant and an additional reducing agent, and the whole preparation process is simple, easy to operate and convenient to popularize and use.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to preparation and application of a composite material of expanded graphite in-situ grown silver nanoparticles.
Background
The preparation of carbon-based noble metal nanoparticle composites currently used for surface enhanced raman spectroscopy can be roughly divided into two categories: reducing noble metal ions attached to the surface of the carbon base by using a reducing agent or an electrochemical method, for example, adding silver nitrate into a modified cellulose solution for chelation in Chinese patent CN113501886A, and then adding a reducing agent for reduction reaction to obtain a cellulose nano-silver composite material; for example, chinese patent CN110016700B utilizes an electrochemical workstation to perform an electrochemical reaction to prepare an enhanced raman substrate with silver-plated surface. Secondly, the independently prepared noble metal nano particles are attached through the interaction with the carbon-based material, and for example, the method for preparing the silver-loaded expanded graphite by using the extra-large scale graphite as proposed in the Chinese patent CN106860904B is the second method. However, in either of the above methods, various chemical reagents need to be introduced, and the prepared composite material needs to be washed if used for surface enhanced raman trace substance detection so as to reduce background signal interference.
Disclosure of Invention
The invention aims to provide a preparation method and application of a composite material of expanded graphite in-situ grown silver nanoparticles.
In order to solve the technical problems, the invention is realized by the following technical scheme:
preparing silver/expanded graphite composite materials with different shapes by adjusting a temperature control program, an inert atmosphere and a raw material ratio; and a substrate with high surface enhanced Raman activity is constructed by utilizing the excellent adsorption characteristic of the expanded graphite and the electromagnetic field enhancement effect of the expanded graphite and the silver. Silver acetate is decomposed at high temperature to generate silver simple substance, so that the composite material of the expanded graphite in-situ loaded with silver nano particles is prepared in an inert atmosphere by a mechanochemical synthesis method. The whole composite material is simple in preparation process and easy to operate, does not need to add a reducing agent or a surfactant, and can be directly used for a surface enhanced Raman scattering substrate to detect trace substances. And the material is designed based on expanded graphite, has good adsorbability, and can enrich the object to be detected.
Specifically, the preparation method of the composite material of the expanded graphite in-situ growth silver nanoparticles comprises the following steps:
(1) ultrasonically washing the expanded graphite for one time;
(2) putting the cleaned expanded graphite and silver acetate into a mortar for grinding;
(3) and (3) placing the ground mixture into a crucible boat, and heating the crucible boat in a tube furnace to 300 ℃ in an inert atmosphere until the mixture is calcined for 2-4 hours to obtain a sample.
Furthermore, the ultrasonic washing time of the expanded graphite in the step (1) is 15-150 min, so that redundant chemical reagents adsorbed on the surface of the expanded graphite in the preparation process of the chemical oxidation method are removed.
Further, the molar mass ratio of the silver acetate to the expanded graphite in the step (2) is 2-30%.
Further, the mortar in the step (2) is an agate mortar to reduce sample loss; the grinding time is about 15min to 1 h.
Further, in the step (3), the preparation of the material is completed in an inert atmosphere, and the used inert gas comprises nitrogen and argon.
Further, the temperature rise program in the step (3) is set to be 5 ℃/min, the calcination is carried out for 2-4 hours at the temperature of 300 ℃ so that the silver acetate is completely decomposed into silver simple substances, and the silver nano particles are uniformly dispersed on the surface of the expanded graphite.
The application of the composite material of the expanded graphite in-situ growth silver nanoparticles comprises the steps of immersing a prepared sample in a trace amount of solution of an object to be detected, taking out the sample after a certain time, and detecting the sample by using a Raman spectrometer.
Further, in the application of the material, the time for the silver/expanded graphite composite material to adsorb the object to be detected is 15 min-2 h.
Further, in the application of the material, a Raman spectrometer is used for detection, and the wavelength of an excitation light of the Raman spectrometer is 638 nm.
The invention has the following beneficial effects:
the preparation method of the composite material for in-situ growth of the silver nanoparticles by the expanded graphite can be used for large-scale commercial production, and has the advantages of simple whole process, easy mastering and low cost. And no other surfactant or reducing agent is introduced in the process of growing the silver particles on the surface of the expanded graphite, so that the background signal interference in the detection of trace substances is reduced. Because the expanded graphite has excellent adsorption characteristics, the expanded graphite has good enrichment and separation effects in trace or trace substance detection and pollutant removal. In addition, the expanded graphite and the silver particles can generate electromagnetic field enhancement, and a high-activity enhanced substrate with a surface enhanced Raman scattering signal can be prepared.
Drawings
FIG. 1 is a microstructure of the 5 mol% silver/expanded graphite composite prepared in example 1.
FIG. 2 is a microstructure of the 10 mol% silver/expanded graphite composite prepared in example 2.
FIG. 3 is the surface enhanced Raman scattering detection spectrum of the solution with 500 ppb crystal violet content in example 2.
FIG. 4 is the surface enhanced Raman scattering detection spectrum of the solution with 500 ppb methylene blue content in example 3.
Detailed Description
The technical solution of the present invention is described in detail and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1
The preparation method of the composite material of the expanded graphite in-situ growth silver nanoparticles comprises the following steps:
step 1, dispersing 200 mg of expanded graphite in 400 ml of water, ultrasonically oscillating for 2 hours, and then drying at 60 ℃ for later use;
step 2, putting 5 mol% of silver acetate and the cleaned expanded graphite into an agate mortar for grinding for 15 min;
step 3, placing the ground mixture into a crucible boat, calcining the mixture for 2 hours in a tubular furnace at 300 ℃ in the nitrogen atmosphere, wherein the heating rate is 5 ℃/min, and the micro-morphology of the calcined material is shown in the attached drawing 1;
the application of the composite material of the expanded graphite in-situ growth silver nano particles comprises the following steps:
2 mg of the sample prepared in step 3 was immersed in 1 mL of a 500 ppb crystal violet solution and taken out after 15 min. And performing SERS characterization on the soaked silver/expanded graphite composite material by using a Raman spectrometer, wherein the wavelength of the used excitation light is 638 nm. The surface enhanced raman spectrum showed characteristic peak positions of crystal violet.
Example 2
The preparation method of the composite material of the expanded graphite in-situ growth silver nanoparticles comprises the following steps:
step 1, dispersing 200 mg of expanded graphite in 400 ml of water, ultrasonically oscillating for 2 hours, and then drying at 60 ℃ for later use;
step 2, putting 10 mol% silver acetate and the cleaned expanded graphite into an agate mortar for grinding for 15 min;
step 3, placing the ground mixture into a crucible boat, calcining the mixture for 2 hours in a tubular furnace at 300 ℃ in the nitrogen atmosphere, wherein the heating rate is 5 ℃/min, and the micro-morphology of the calcined material is shown in the attached figure 2;
the application of the composite material of the expanded graphite in-situ growth silver nano particles comprises the following steps:
2 mg of the sample prepared in step 3 was immersed in 1 mL of a 500 ppb crystal violet solution and taken out after 15 min. SERS characterization is carried out on the soaked silver/expanded graphite composite material by using a Raman spectrometer, the wavelength of the used excitation light is 638 nm, and the detection result is shown in figure 3. The surface enhanced raman spectrum showed characteristic peak positions of crystal violet.
Example 3
The preparation method of the composite material of the expanded graphite in-situ growth silver nanoparticles comprises the following steps:
step 1, dispersing 200 mg of expanded graphite in 400 ml of water, ultrasonically oscillating for 2 hours, and then drying at 60 ℃ for later use;
step 2, putting the 10 mol% silver acetate and the cleaned expanded graphite into an agate mortar for grinding for 60 min;
step 3, placing the ground mixture into a crucible boat, calcining for 3 hours at 300 ℃ in a tubular furnace in the nitrogen atmosphere, and raising the temperature at a rate of 5 ℃/min;
the application of the composite material of the expanded graphite in-situ growth silver nano particles comprises the following steps:
2 mg of the sample prepared in step 3 was immersed in 1 mL of 500 ppb methylene blue solution and removed after 20 min. SERS characterization is carried out on the soaked silver/expanded graphite composite material by using a Raman spectrometer, the wavelength of the used excitation light is 638 nm, and the detection result is shown in figure 4. The surface enhanced raman spectrum showed the characteristic peak position of methylene blue.
Example 4
The preparation method of the composite material of the expanded graphite in-situ growth silver nanoparticles comprises the following steps:
step 1, dispersing 200 mg of expanded graphite in 400 ml of water, ultrasonically oscillating for 3 hours, and then drying at 60 ℃ for later use;
step 2, putting 15 mol% of silver acetate and the cleaned expanded graphite into an agate mortar for grinding for 60 min;
step 3, placing the ground mixture into a crucible boat, calcining for 3 hours at 300 ℃ in a tubular furnace under the argon atmosphere, and raising the temperature at a rate of 5 ℃/min;
the application of the composite material of the expanded graphite in-situ growth silver nano particles comprises the following steps:
2 mg of the sample prepared in step 3 was immersed in 1 mL of a 100 ppb crystal violet solution and taken out after 30 min. And performing SERS characterization on the soaked silver/expanded graphite composite material by using a Raman spectrometer, wherein the wavelength of the used excitation light is 638 nm. The surface enhanced raman spectrum showed characteristic peak positions of crystal violet.
Example 5
The preparation method of the composite material of the expanded graphite in-situ growth silver nanoparticles comprises the following steps:
step 1, dispersing 200 mg of expanded graphite in 400 ml of water, ultrasonically oscillating for 2 hours, and then drying at 60 ℃ for later use;
step 2, putting 30 mol% of silver acetate and the cleaned expanded graphite into an agate mortar for grinding for 30 min;
step 3, placing the ground mixture into a crucible boat, calcining for 4 hours at 300 ℃ in a tubular furnace in the nitrogen atmosphere, and raising the temperature at a rate of 5 ℃/min;
the application of the composite material of the expanded graphite in-situ growth silver nano particles comprises the following steps:
2 mg of the sample prepared in step 3 was immersed in 1 mL of a 1 ppm methylene blue solution and taken out after 30 min. And performing SERS characterization on the soaked silver/expanded graphite composite material by using a Raman spectrometer, wherein the wavelength of the used excitation light is 638 nm. The surface enhanced raman spectrum showed the characteristic peak position of methylene blue.
Particularly, the technical scheme of the invention has been subjected to pilot test, namely a small-scale test of the product before large-scale mass production, after the pilot test is finished, user use investigation is carried out in a small range, and the investigation result shows that the user satisfaction is higher, and the preparation of formal production of the product for industrialization, including intellectual property risk early warning investigation, is started.
Claims (8)
1. A preparation method of a composite material of expanded graphite in-situ grown silver nanoparticles is characterized by comprising the following steps:
(1) ultrasonically washing the expanded graphite for one time;
(2) putting the cleaned expanded graphite and silver acetate into a mortar for grinding;
(3) and (3) placing the ground mixture into a crucible boat, and heating the crucible boat in a tube furnace to 300 ℃ in an inert atmosphere until the mixture is calcined for 2-4 hours to obtain a sample.
2. The preparation method of the composite material for in-situ growing of the silver nanoparticles by using the expanded graphite as claimed in claim 1, wherein the molar mass ratio of the silver acetate to the expanded graphite in the step (2) is 2-30%.
3. The method for preparing a composite material of in-situ grown silver nanoparticles from expanded graphite according to claim 1, wherein the inert gas used is nitrogen or argon.
4. The preparation method of the composite material for in-situ growth of silver nanoparticles by using the expanded graphite as claimed in claim 1, wherein the mortar in the step (2) is an agate mortar, and the grinding time is 15 min-1 h.
5. The method for preparing a composite material of in-situ grown silver nanoparticles by using expanded graphite as claimed in claim 1, wherein the temperature rise program in the step (3) is controlled to be 5 ℃/min.
6. The composite of expanded graphite in-situ grown silver nanoparticles of claim 1, wherein the composite is used for surface enhanced raman spectroscopy for trace species detection.
7. The application of the composite material of the silver nanoparticles grown in situ from the expanded graphite as claimed in claim 7, wherein the time for adsorbing the substance to be detected by the silver/expanded graphite composite material is 15 min-2 h.
8. The use of the expanded graphite in-situ grown silver nanoparticle composite material of claim 7, wherein the wavelength of the excitation light of the Raman spectrometer is 638 nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111381652.0A CN114195146A (en) | 2021-11-22 | 2021-11-22 | Preparation method and application of composite material of expanded graphite in-situ grown silver nanoparticles |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117686480A (en) * | 2024-01-24 | 2024-03-12 | 深圳北理莫斯科大学 | Preparation method and application of high-performance flexible surface-enhanced Raman substrate |
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2021
- 2021-11-22 CN CN202111381652.0A patent/CN114195146A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| SAGAR KUMAR NAYAK1等: "Silver (Ag) nanoparticle‑decorated expanded graphite (EG) epoxy composite: evaluating thermal and electrical properties", 《JOURNAL OF MATERIALS SCIENCE》, pages 20574 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117686480A (en) * | 2024-01-24 | 2024-03-12 | 深圳北理莫斯科大学 | Preparation method and application of high-performance flexible surface-enhanced Raman substrate |
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Application publication date: 20220318 |