Porous graphite-silver nano-diamond composite as well as preparation method and application thereof

A technology of porous graphene and composite materials, applied in the field of porous graphene-silver nano-square composite materials and its preparation, can solve the problem of limiting the physical enhancement of silver nano-squares, the inability to selectively detect thiram series pesticides, and the inability to obtain selectivity To accurately detect the SERS active substrate and other issues, to achieve the effect of simple preparation method and reduced preparation cost

Active Publication Date: 2017-03-22
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this product can be used as an active substrate for surface-enhanced Raman scattering, a laser Raman spectrometer is used to measure the content of rhodamine 6G or polychlorinated biphenyl PCB-3 or methyl parathion attached thereon, but it is different from its preparation method. There are deficiencies. First, the product cannot selectively detect thiram series pesticides; secondly, the preparation method can not obtain the SERS active substrate for selectively detecting thiram series pesticides; Assembly and adsorption of silver nanocubes on the graphene pore walls, so that the silver nanocubes are densely packed and the surface is wrapped by graphene, which greatly limits the physical enhancement of silver nanocubes

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  • Porous graphite-silver nano-diamond composite as well as preparation method and application thereof
  • Porous graphite-silver nano-diamond composite as well as preparation method and application thereof
  • Porous graphite-silver nano-diamond composite as well as preparation method and application thereof

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Effect test

Embodiment 1

[0036] The concrete steps of preparation are:

[0037] Step 1: First, according to the weight ratio of graphene oxide, sodium bisulfite and deionized water as 1:480:135, the three are mixed and ultrasonically oscillated for 5 minutes to obtain a mixed solution. Then the mixed solution was placed at 90° C. for 4 h, and after cooling, a black graphene gel suspended in water was obtained.

[0038] In step 2, the black graphene gel was rinsed once with deionized water and then freeze-dried; wherein, the freeze-drying temperature was -6°C and the time was 30 hours to obtain spongy porous graphene. Then according to the weight ratio of the ethanol dispersion of spongy porous graphene and 0.1wt% silver nano-squares is the ratio of 1:30000, the spongy porous graphene is immersed in the ethanol dispersion of silver nano-squares for 0.5h and then taken out to obtain mid product.

[0039] Step 3, the intermediate product is placed at 30 ℃ and dried first, and then the dried intermediat...

Embodiment 2

[0041] The concrete steps of preparation are:

[0042] Step 1: First, according to the weight ratio of graphene oxide, sodium bisulfite and deionized water as 1:490:130, the three are mixed and then ultrasonically oscillated for 6 minutes to obtain a mixed solution. Then the mixture was placed at 93° C. for 3.5 h, and after cooling, a black graphene gel suspended in water was obtained.

[0043] In step 2, the black graphene gel was rinsed twice with deionized water and then freeze-dried; wherein, the freeze-drying temperature was -9.5° C. and the time was 24 hours to obtain spongy porous graphene. Then according to the weight ratio of the ethanol dispersion of spongy porous graphene and 0.3wt% silver nano-squares is the ratio of 1:23250, after spongy porous graphene is immersed in the ethanol dispersion of silver nano-squares for 0.8h, it is taken out to obtain mid product.

[0044] Step 3, the intermediate product is placed at 35 ℃ and dried first, and then the dried interm...

Embodiment 3

[0046] The concrete steps of preparation are:

[0047] Step 1: First, according to the weight ratio of graphene oxide, sodium bisulfite and deionized water as 1:500:125, the three are mixed and ultrasonically oscillated for 8 minutes to obtain a mixed solution. Then the mixture was placed at 95° C. for 3 h, and after cooling, a black graphene gel suspended in water was obtained.

[0048] Step 2, the black graphene gel was first rinsed with deionized water for 3 times and then freeze-dried; wherein, the freeze-drying temperature was -13°C and the time was 18 hours to obtain spongy porous graphene. Then according to the weight ratio of the ethanol dispersion liquid of spongy porous graphene and 0.6wt% silver nano-squares is the ratio of 1:16500, the spongy porous graphene is immersed in the ethanol dispersion liquid of silver nano-squares for 1h and then taken out to obtain the intermediate product.

[0049] Step 3, the intermediate product is first dried at 40°C, and then the...

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Abstract

The invention discloses a porous graphite-silver nano-diamond composite as well as a preparation method and an application thereof. The composite comprises porous graphite and a silver nano-diamonds, wherein pores of the porous graphite are intercommunicated micropores, and one side of the silver nano-diamond is in adsorption connection with the pore walls of the porous graphite. According to the preparation method, graphene oxide, sodium bisulfite and deionized water are mixed and subjected to ultrasonic oscillation, an obtained mixed solution is left to stand at 90-100 DEG C and cooled, black graphene gel suspended in water is rinsed with deionized water and subjected to freeze drying, obtained spongy porous graphene is soaked in an ethyl alcohol dispersion solution of the silver nano-diamond and taken out, an intermediate product is obtained, then the dried intermediate product is compressed, and the target product is prepared. The composite is quite suitable for serving as an active substrate for SERS (surface-enhanced Raman scattering), so that a laser Raman spectrometer selectively measures the content of dimethyldithiocarbamate pesticides attached to the composite.

Description

technical field [0001] The invention relates to a composite material and its preparation method and application, in particular to a porous graphene-silver nano-square composite material and its preparation method and application. Background technique [0002] Surface-enhanced Raman scattering (SERS) spectroscopy is the vibrational spectrum of molecules, which can provide molecular fingerprint information and has extremely high sensitivity. Therefore, SERS analysis technology has a wide range of applications in the fields of chemistry, biology, medicine, environment and food safety. At present, people have made various efforts to develop different SERS materials, such as a noble metal nanoparticle-porous graphene composite material and its preparation method published by the applicant on July 8, 2015 in the Chinese invention patent application CN104759616A and uses. The composite material mentioned in the patent application documents for this invention is porous graphene wi...

Claims

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Application Information

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IPC IPC(8): G01N21/65G01N23/22
CPCG01N21/658G01N23/22
Inventor 朱储红孟国文王秀娟
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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