Cu2Se-Pd hybrid material as well as preparation method and application thereof

A hybrid material, C2H5 technology, used in chemical instruments and methods, nanotechnology for materials and surface science, material excitation analysis, etc., to achieve the effects of short time, convenient response value, and low reaction temperature

Inactive Publication Date: 2014-08-27
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Pd and Cu 2 Se is combined as a SERS substrate, which has not been reported before
[0005] On the other hand, in the method for detecting 4-mercaptopyridine (4-Mpy) based on SERS, the SERS substrate mainly includes metal nanocrystals (such as Au, Ag, Pd, etc.), semiconductor oxides and sulfides (such as: CuO, Fe 2 o 3 , ZnO, Ag 2 S, ZnS, etc.), while reports on semiconductor selenides or their composite materials are rarely published in public reports

Method used

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  • Cu2Se-Pd hybrid material as well as preparation method and application thereof
  • Cu2Se-Pd hybrid material as well as preparation method and application thereof
  • Cu2Se-Pd hybrid material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] At room temperature, in a clean and dry 100mL three-necked flask, add 0.23g precursor [(C 2 h 5 ) 4 N] 2 [CuCl 4 ] solid, 10 mL DMPU and 1 mL LUA. Then, the above mixture was heated at 5 °C min -1 The heating rate was heated to 180°C, and kept at this temperature for 20-40min, and then 5mL of selenium solution (0.05g SeO 2 and 5mL terpineol mixed solution), after incubation for 1h, the hexagonal phase CuSe microcrystals were obtained after separation and washing. Mix the obtained CuSe and 12mLTOP, keep it at 200-250°C for 1h, interact to obtain monoclinic Cu 2 Se, separated and washed to obtain monoclinic phase Cu 2 Se microcrystals; further Cu 2 Se microcrystals and 0.02g Pd(NO 3 ) 2 2H 2 0. 15mL isopropanol was mixed, stirred at room temperature for 30min, after washing with ethanol and drying, the target product Cu 2 Se-Pd microcrystals. The object was vacuum dried at 40°C for analysis and characterization.

[0042] Use EDX and mapping test to analyze t...

Embodiment 2

[0048] At room temperature, in a clean and dry 100mL three-necked flask, add 0.23g of [(C 2 h 5 ) 4 N] 2 [CuCl 4 ] solid, 10mL DMPU and 1mL LUA, and 5mL selenium solution (0.05g SeO 2 and 5mL terpineol mixture) were directly added to the reaction system. Then the above mixture was heated at 5°C min -1 The heating rate was heated to 180°C, and after being kept at this temperature for 1h, the cubic phase Cu was obtained after centrifugation and washing. 2-X Se microcrystals; the resulting Cu 2-X Se and 12mLTOP are mixed and incubated at 200-250°C for 1h to interact to obtain monoclinic phase Cu 2 Se, separated and washed to obtain monoclinic phase Cu 2 Se microcrystals; it was further mixed with 0.02g Pd(NO 3 ) 2 2H 2 0. 15mL isopropanol was mixed, stirred at room temperature for 30min, after washing with ethanol and drying, the target product Cu 2 Se-Pd microcrystals. Then the object was dried under vacuum at 40°C for analysis and characterization.

[0049] Use ED...

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Abstract

The invention discloses a preparation method of a Cu2Se-Pd hybrid material and a prepared material. A copper source is tetrachloro cupric (II) acid tetraethylammonium, and a selenium source is a mixed liquid formed by dissolving SeO2 into terpilenol. The preparation method comprises the following steps: performing reaction in DMPU (dimethyl propyl urea) to obtain hexagonal phase CuSe or cubic phase Cu2-XSe by virtue of adopting a solid-liquid phase synthetic method; further extracting a product by virtue of TOP to obtain mono-clinic phase Cu2Se; compounding the mono-clinic phase Cu2Se with noble metal Pd to prepare the Cu2Se-Pd hybrid material. The method disclosed by the invention can be used for synthesizing the nano-level Cu2Se-Pd hybrid material under normal pressure and relatively low temperature, and is simple in process and short in reaction time; the prepared hybrid material can be used as an SERS (surface enhanced raman spectroscopy) substrate so as to be applied to SERS detection 4-Mpy, and is strong in response signal and high in selectivity; the limit of detection can reach 10<-9>molL<-1>. Compared with independent semiconductor Cu2Se and metal Pd, the Cu2Se-Pd hybrid material shows more excellent SERS performances.

Description

technical field [0001] The present invention relates to a Cu 2 Se-Pd micron-scale hybrid material and its preparation method, and the application of the hybrid material on surface-enhanced Raman spectroscopy (SERS). Background technique [0002] The surface-enhanced Raman effect was discovered in 1974. Fleishmann et al. found a very strong Raman spectrum signal in pyridine adsorbed on the surface of a rough silver electrode, and called this phenomenon the surface-enhanced Raman effect (SERS). Subsequently, Van Duyne, Gersten and Kerker conducted in-depth basic research and theoretical discussions on this phenomenon. Surface-enhanced Raman spectroscopy itself has the characteristics of high sensitivity, large response value, non-destructive testing, and simple pretreatment. After entering the 1990s, with the vigorous development of nanotechnology, a variety of optional materials were provided for the surface-enhanced Raman spectroscopy substrate, which further promoted the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/00B82Y30/00B82Y40/00G01N21/65
Inventor 包建春张龙韩敏戴志晖
Owner NANJING NORMAL UNIVERSITY
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