Fluorescence-enhanced nano-probes and preparation method thereof, and optical microscope imaging method of rock micro-nano pore

Abstract

The invention discloses fluorescence-enhanced nano-probes and a preparation method thereof, and an optical microscope imaging method of rock micro-nano pores. Each nano-probe comprises a nano-particle, a silicon dioxide modified layer and fluorochrome; the silicon dioxide modified layer is attached to the surface of the nano-particle; the fluorochrome is bound to the surface of the silicon dioxidemodified layer. The optical microscope imaging method of rock micro-nano pores comprises the following steps: injecting the fluorescence-enhanced nano-probe into cracks and pores of the rock; and performing optical microscope imaging on the pores, filled with the fluorescence-enhanced nano-probes, of the rock. The fluorescence-enhanced nano-probes are injected into the rock, the fluorescence molecules are hard to escape and have obvious color difference from the rock matrix and the cement; the identification on the pores and the throat are extremely favorable under the optical microscope; andthe fluorescence-enhanced nano-probes can be used for a long time without considering the influence of the weakening of the fluorescence along the time, and the pore structure of the rock can be accurately and conveniently reflected for a long time.

Description

technical field

[0001] The invention relates to the fields of geological resources and geological engineering, in particular to a fluorescence-enhanced nanometer probe, a preparation method thereof, and an optical microscope imaging method for rock micro-nano pores. Background technique

[0002] The characterization of rock pore structure is the basis for the fine description of geological resources, and plays a guiding role in correctly understanding the characteristics of rock reservoirs. At the same time, it plays a decisive role in correctly understanding geological resources and their efficient and rational development. The existing materials that use composite nanoparticles to characterize the rock pore structure are mainly synthesized by coating method. The implementation process is to disperse nanoparticles and dye molecules in tetraethyl silicate (TEOS) solution, and then add absolute ethanol to make them TEOS is decomposed into a substance similar to a network stru...

Examples

preparation example Construction

[0030] Some embodiments of the present invention also provide a method for preparing the above-mentioned fluorescence-enhanced nanoprobe, which includes: reacting the nanoparticle with a silicon dioxide modified layer on the surface with the fluorescent dye to make the fluorescence A dye is bound to the silica modified layer.

[0031] Specifically, in some embodiments, nanoparticles with a modified layer of silicon dioxide on the surface are prepared through the following steps: preparing nanoparticles by co-precipitation; attaching a silicon dioxide layer to the surface of the nanoparticles, and removing the silicon dioxide layer Surface modification is performed to form a silicon dioxide modified layer. In some embodiments, the silicon dioxide layer is modified by modifying the surface of the silicon dioxide layer with amino groups through a surface chemical modifier, wherein the fluorescent dye is rhodamine B.

[0032]Further, in some embodiments, the surface chemical modi...

Embodiment 1

[0049] Accurately weigh 2.34g FeCl 3 ·6H 2 O (0.01mol) and 0.96g FeCl 2 4H 2 O (0.005mol) in a three-necked flask, add 100mL deionized water (nitrogen to remove oxygen) and stir to dissolve, put it in a constant temperature water bath and heat the temperature to 80 ° C, under the protection of nitrogen and mechanical stirring, add to the mixed solution Slowly add 40mL of 1.15mol / L NaOH solution dropwise into the solution, after the dropwise addition is completed, add 40mL of 0.1mol / L trisodium citrate as a surfactant, stir at a constant temperature of 80°C for 0.5h, and decant the synthesized Fe 3 o 4 Nanoparticles are separated from the reaction system. Fe will be prepared 3 o 4 Nanoparticles were redispersed in 80% ethanol solution, adding 5mL NH 3 ·H 2 After O, under the protection of nitrogen and mechanical stirring, the TEOS ethanol solution (V TEOS / V 无水乙醇 =1 / 10) 33mL, continue to stir the reaction for 2h. After washing with ethanol several times, the reactio...

Embodiment 2

[0052] Accurately weigh 2.00g Fe 2 (SO 4 ) 3 (0.005mol) with 0.76g FeSO 4 (0.005mol) in a three-necked flask, add 100mL deionized water (nitrogen to remove oxygen) and stir to dissolve, put it into a constant temperature water bath and heat the temperature to 80 ° C, under the protection of nitrogen and mechanical stirring, add to the mixed solution Slowly add 40mL of 1.15mol / L NaOH solution dropwise. After the dropwise addition is completed, add 40mL of 0.1mol / L trisodium citrate as a surfactant, stir at a constant temperature of 80°C for 0.5h, and decant the synthesized Fe 3 o 4Nanoparticles are separated from the reaction system. Fe will be prepared 3 o 4 Nanoparticles were redispersed in 80% ethanol solution, adding 5mL NH 3 ·H 2 After O, under the protection of nitrogen and mechanical stirring, the TEOS ethanol solution (V TEOS / V 无水乙醇 =1 / 10) 55mL, continue to stir the reaction for 2h. After washing with ethanol several times, the reaction product was obtained....

technical field

[0001] The invention relates to the fields of geological resources and geological engineering, in particular to a fluorescence-enhanced nanometer probe, a preparation method thereof, and an optical microscope imaging method for rock micro-nano pores. Background technique

[0002] The characterization of rock pore structure is the basis for the fine description of geological resources, and plays a guiding role in correctly understanding the characteristics of rock reservoirs. At the same time, it plays a decisive role in correctly understanding geological resources and their efficient and rational development. The existing materials that use composite nanoparticles to characterize the rock pore structure are mainly synthesized by coating method. The implementation process is to disperse nanoparticles and dye molecules in tetraethyl silicate (TEOS) solution, and then add absolute ethanol to make them TEOS is decomposed into a substance similar to a network stru...

Examples

preparation example Construction

[0030] Some embodiments of the present invention also provide a method for preparing the above-mentioned fluorescence-enhanced nanoprobe, which includes: reacting the nanoparticle with a silicon dioxide modified layer on the surface with the fluorescent dye to make the fluorescence A dye is bound to the silica modified layer.

[0031] Specifically, in some embodiments, nanoparticles with a modified layer of silicon dioxide on the surface are prepared through the following steps: preparing nanoparticles by co-precipitation; attaching a silicon dioxide layer to the surface of the nanoparticles, and removing the silicon dioxide layer Surface modification is performed to form a silicon dioxide modified layer. In some embodiments, the silicon dioxide layer is modified by modifying the surface of the silicon dioxide layer with amino groups through a surface chemical modifier, wherein the fluorescent dye is rhodamine B.

[0032]Further, in some embodiments, the surface chemical modi...

Embodiment 1

[0049] Accurately weigh 2.34g FeCl 3 ·6H 2 O (0.01mol) and 0.96g FeCl 2 4H 2 O (0.005mol) in a three-necked flask, add 100mL deionized water (nitrogen to remove oxygen) and stir to dissolve, put it in a constant temperature water bath and heat the temperature to 80 ° C, under the protection of nitrogen and mechanical stirring, add to the mixed solution Slowly add 40mL of 1.15mol / L NaOH solution dropwise into the solution, after the dropwise addition is completed, add 40mL of 0.1mol / L trisodium citrate as a surfactant, stir at a constant temperature of 80°C for 0.5h, and decant the synthesized Fe 3 o 4 Nanoparticles are separated from the reaction system. Fe will be prepared 3 o 4 Nanoparticles were redispersed in 80% ethanol solution, adding 5mL NH 3 ·H 2 After O, under the protection of nitrogen and mechanical stirring, the TEOS ethanol solution (V TEOS / V 无水乙醇 =1 / 10) 33mL, continue to stir the reaction for 2h. After washing with ethanol several times, the reactio...

Embodiment 2

[0052] Accurately weigh 2.00g Fe 2 (SO 4 ) 3 (0.005mol) with 0.76g FeSO 4 (0.005mol) in a three-necked flask, add 100mL deionized water (nitrogen to remove oxygen) and stir to dissolve, put it into a constant temperature water bath and heat the temperature to 80 ° C, under the protection of nitrogen and mechanical stirring, add to the mixed solution Slowly add 40mL of 1.15mol / L NaOH solution dropwise. After the dropwise addition is completed, add 40mL of 0.1mol / L trisodium citrate as a surfactant, stir at a constant temperature of 80°C for 0.5h, and decant the synthesized Fe 3 o 4Nanoparticles are separated from the reaction system. Fe will be prepared 3 o 4 Nanoparticles were redispersed in 80% ethanol solution, adding 5mL NH 3 ·H 2 After O, under the protection of nitrogen and mechanical stirring, the TEOS ethanol solution (V TEOS / V 无水乙醇 =1 / 10) 55mL, continue to stir the reaction for 2h. After washing with ethanol several times, the reaction product was obtained....

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