CN109648096B - Method for converting random nanocone array into silver nanosheet constructed micro/nano structure array in situ - Google Patents
Method for converting random nanocone array into silver nanosheet constructed micro/nano structure array in situ Download PDFInfo
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Abstract
The invention discloses a method for converting any nanocone array into a micro/nano structure array constructed by silver nanosheets in situ, wherein a layer of copper film is sputtered on the surface of any nanocone array to obtain a copper array; soaking the copper array in a copper salt solution by utilizing a centering reaction between copper and the copper salt solution, and obtaining a cuprous oxide array after the reaction; and (3) soaking the cuprous oxide array in a solution containing silver nitrate, and reacting to obtain the micro/nano structure array constructed by the silver nano sheets. The array structure can be obtained without the limitation of the substrate. The structure has the high specific surface area of the nano-sheet, provides more active sites, and simultaneously, the array structure can ensure the uniformity and stability of a sample.
Description
Technical Field
The invention relates to a method for in-situ conversion of a micro/nano structure array, in particular to a method for in-situ conversion of any nano cone array into a micro/nano structure array constructed by silver nano sheets.
Background
The noble metal nano-particles or micro/nano-structured particles have stronger SERS activity and higher structural stability. Furthermore, to ensure good reproducibility of SERS measurements, the micro/nano structured particles need to be ordered. The micro/nano structure array constructed by the nano sheets generates more hot spots because of the existence of many sharp edges. The preparation method of the plasma nanosheet is various, such as an electrochemical deposition method, a galvanic couple replacement method and Cu2The O template method, etc.
The problems encountered in the current research are mainly the following two:
(1) can easily utilize Cu2Micro-nano structure assembled by preparing Ag nanosheets from OHowever, it is difficult to prepare such a method into an array;
(2) the method for preparing the array structure has certain limitation, and the existing method only can utilize an electrochemical deposition method to prepare a micro/nano structure array constructed by silver nano sheets on a conductive substrate, so that the method is limited.
Disclosure of Invention
The invention aims to provide a method for converting any nanocone array into a micro/nano structure array constructed by silver nano sheets in situ.
The purpose of the invention is realized by the following technical scheme:
the method for in-situ conversion of any nanocone array into a micro/nano structure array constructed by silver nano sheets comprises the following steps:
(1) preparing a single-layer film of PS balls which are arranged closely and self-assembled on the surface of a clean substrate by a gas-liquid interface self-assembly method;
(2) method of etching with reactive ions, using SF6Etching the substrate with the surface provided with the PS ball array by using gas to obtain any nano cone array structure;
(3) sputtering a layer of copper film on the surface of any nanocone array by using a magnetron sputtering method to obtain a copper array;
(4) soaking the copper array in a copper salt solution by utilizing a centering reaction between copper and the copper salt solution, and obtaining a cuprous oxide array after the reaction;
(5) and (3) soaking the cuprous oxide array in a solution containing silver nitrate, and reacting to obtain the micro/nano structure array constructed by the silver nano sheets.
According to the technical scheme provided by the invention, the method for converting any nano-cone array into the micro/nano-structure array constructed by the silver nano-sheets in situ is based on Cu2The O in-situ conversion method comprises the steps of in-situ conversion on the surface of any nano-cone array to obtain particles assembled by nano sheets, further assembling the particles to obtain an array, and preparing a micro/nano structure array assembled by Ag nano sheets on a non-conductive substrate, wherein the micro/nano structure array can obtain an array structure without being influenced by the structure of the Ag nano sheetsTo the substrate. The structure has the high specific surface area of the nano-sheet, provides more active sites, and simultaneously, the array structure can ensure the uniformity and stability of a sample.
Drawings
FIG. 1 is a scanning electron micrograph of a 1000nm PS ball array on a silicon substrate surface by a gas-liquid interface self-assembly method according to an embodiment of the present invention;
FIG. 2 is a scanning electron micrograph of a silicon array obtained by etching a 1000nm PS array according to an embodiment of the present invention;
FIG. 3 is a scanning electron microscope photograph of a copper film obtained on the surface of a silicon array by magnetron sputtering in an embodiment of the present invention;
FIG. 4 is a scanning electron micrograph of a copper array converted to a cuprous oxide array using a centering reaction in an example of the invention (inset is an enlargement of a single particle);
fig. 5 is a scanning electron microscope photograph of a micro/nano-structured array constructed by converting a cuprous oxide array into silver nano-sheets in an embodiment of the present invention.
Detailed Description
The embodiments of the present invention will be described in further detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art.
The method for converting any nanocone array into the micro/nano structure array constructed by the silver nanosheets in situ has the preferred specific implementation mode that:
the method comprises the following steps:
(1) preparing a single-layer film of PS balls which are arranged closely and self-assembled on the surface of a clean substrate by a gas-liquid interface self-assembly method;
(2) method of etching with reactive ions, using SF6Etching the substrate with the surface provided with the PS ball array by using gas to obtain any nano cone array structure;
(3) sputtering a layer of copper film on the surface of any nanocone array by using a magnetron sputtering method to obtain a copper array;
(4) soaking the copper array in a copper salt solution by utilizing a centering reaction between copper and the copper salt solution, and obtaining a cuprous oxide array after the reaction;
(5) and (3) soaking the cuprous oxide array in a solution containing silver nitrate, and reacting to obtain the micro/nano structure array constructed by the silver nano sheets.
The step (1) comprises the following steps:
firstly, PS balls with the diameter of 120-1000 nm are selected, dispersed in deionized water and ethanol, and then subjected to ultrasonic treatment to uniformly disperse the PS balls. The PS beads were then dropped onto the surface of a clean slide with water added to the surface to form a monolayer. After a period of drying, the coverslip was transferred to a beaker filled with water, at which time the PS sphere monolayer would float to the surface of the water. Fishing up the PS ball array of a water interface and an air interface by using a clean substrate of 1cm multiplied by 1cm, namely transferring the PS ball array to the surface of a substrate to obtain a closely-arranged PS ball single-layer film array, wherein the clean substrate is a silicon, glass, polytetrafluoroethylene or PE film;
the step (2) comprises the following steps:
and etching the substrate by taking the PS ball array as a mask, wherein the specific experimental parameters are as follows: the current is 0.5-5A, the pressure is 0.05-0.50 Pa, the flow rate of sulfur hexafluoride gas is 10-50 sccm, the power is 100-500 w, and the etching time is 30 s-9 min;
in the step (3), the specific experimental parameters are as follows:
the vacuum degree is 10-70 mTorr, the sputtering current is 15-90 mA, and the sputtering time is 2-30 min;
in the step (4), the copper salt includes copper nitrate, copper sulfate and/or copper acetate, and specifically includes:
preparing a copper salt solution: dissolving 0.0200-1.0000 g of copper salt into 10-100 mL of deionized water to obtain a precursor solution of copper;
then, soaking the nanocone array with the copper film covered on the surface in a precursor solution of copper, and setting the soaking time to be 10-30 min;
after the reaction is finished, taking out the substrate, and alternately cleaning the substrate for a plurality of times by using deionized water and absolute ethyl alcohol to obtain a cuprous oxide array;
with N2Drying to obtain a cuprous oxide array for the next reaction;
the step (5) comprises:
preparing a silver nitrate reaction solution: dispersing 0.0100-0.3000 g of silver nitrate, 0.0100-1.0000 g of anhydrous sodium citrate and 5-50 uL of concentrated nitric acid into 5-50 mL of deionized water, and then placing a 1cm x 1cm cuprous oxide substrate into the mixed solution to soak for 1-30 min;
after the reaction is finished, the substrate is taken out and is alternately cleaned for a plurality of times by deionized water and absolute ethyl alcohol.
In the step (1), the size of the PS ball is 1000nm, and the substrate is a silicon wafer.
In the step (2), the current is 3A, the pressure is 0.1Pa, the flow rate of sulfur hexafluoride gas is 36sccm, the power is 200w, and the etching time is 7 min.
In the step (3), the vacuum degree is 35mTorr, the sputtering current is 40mA, and the sputtering time is 5 min.
In the step (4), 0.4000g of anhydrous copper sulfate (CuSO)4) Dissolving into 50mL of deionized water to obtain a copper sulfate solution, and setting the soaking time to be 30 min.
In the step (5), 0.0306g of silver nitrate, 0.0352g of anhydrous sodium citrate and 10uL of concentrated nitric acid are dispersed into 20mL of deionized water, and then a 1cm × 1cm cuprous oxide substrate is placed in the mixed solution for 30 min.
According to the method for converting any nano-cone array into the micro/nano-structure array constructed by the silver nano-sheets in situ, the obtained product is an array structure obtained by further assembling particles constructed by the silver nano-sheets. The traditional method for preparing the micro/nano structure array constructed by the nano sheets is an electrochemical deposition method, and is limited to preparing the structure on a conductive silicon substrate, but the method can prepare the silver nano sheet constructed micro/nano structure array on any substrate capable of obtaining a cone array. The structure comprises the advantages of a sheet structure and a double layer of an array structure, on one hand, the sheet structure has larger specific surface area and can provide more active sites when being contacted with test molecules; on the other hand, due to the array structure, the uniformity of the structure and the stability of the test result can be ensured, so that the structure has more excellent performance.
According to the invention, the micro/nano structure array constructed by the silver nano sheets can be prepared through in-situ conversion on the surface of any substrate capable of obtaining the nano cone array by using an in-situ conversion method and a chemical reaction. The structure has a sheet structure, can have larger specific surface area and provides more active sites, and is more stable, more uniform and more excellent in performance compared with a dispersed particle structure.
The specific embodiment is as follows:
example 1
The method for converting any arbitrary nanocone array into a micro/nano-structure array constructed by silver nanosheets in situ, described in this example 1, includes the following steps:
(1) and preparing a tightly arranged PS ball self-assembled single-layer film on the surface of the clean silicon substrate by using a gas-liquid interface self-assembly method. A tightly packed array of PS sphere monolayers was obtained on a 1cm by 1cm clean silicon substrate surface, with PS spheres of 1000nm diameter selected, as shown in FIG. 1.
(2) Method of etching with reactive ions, using SF6And etching the silicon substrate with the PS ball array on the surface by using the gas to obtain the silicon array. The specific experimental parameters were: the current is 3A, the pressure is 0.1Pa, the flow rate of the gas is 36sccm, the power is 200w, the etching time is 7min, and the appearance of the silicon array is shown in FIG. 2.
(3) And sputtering a layer of copper film on the surface of the silicon array by using a magnetron sputtering method to obtain the copper array. The specific experimental parameters were: the degree of vacuum was 35mTorr, the magnitude of sputtering current was 40mA, and the sputtering time was 5min, and an array with a surface-coated copper film was obtained as shown in FIG. 3.
(4) And (3) soaking the copper array in a copper salt solution, and reacting to obtain the cuprous oxide array. First 0.4000g of copper nitrate [ Cu (NO)3)2]Dissolved in 50mL of deionized water to obtain a copper nitrate solution. And (3) soaking the array covered with the copper film on the surface in the prepared copper nitrate solution for 30min, and after the reaction is finished, taking out the substrate to obtain a cuprous oxide array, as shown in figure 4. Then alternately cleaning with deionized water and anhydrous ethanol for several timesN2And standing for later use after blow-drying.
(5) And (3) soaking the cuprous oxide array in a solution containing silver nitrate, and reacting to obtain the micro/nano structure array constructed by the silver nano sheets. Preparing a silver nitrate reaction solution: 0.0306g of silver nitrate, 0.0352g of anhydrous sodium citrate, and 10uL of concentrated nitric acid were dispersed in 20mL of deionized water, after which a 1cm × 1cm cuprous oxide substrate was placed in the mixed solution for 30 min. After the reaction is finished, taking out the substrate, alternately cleaning the substrate for a plurality of times by using deionized water and absolute ethyl alcohol, and using N2After drying, a micro/nano structure array constructed by silver nano sheets prepared based on in-situ conversion of the silicon array is obtained, as shown in fig. 5.
Example 2
The method for converting any arbitrary nanocone array into a micro/nano-structure array constructed by silver nanosheets in situ, described in this embodiment 2, includes the following steps:
(1) a gas-liquid interface self-assembly method is utilized to prepare a tightly arranged PS ball self-assembly single-layer film on the surface of a clean polytetrafluoroethylene substrate. PS spheres with the diameter of 1000nm are selected, and a closely-arranged PS sphere single-layer film array is obtained on the surface of a clean polytetrafluoroethylene substrate with the thickness of 1cm multiplied by 1 cm.
(2) Method of etching with reactive ions, using SF6And etching the polytetrafluoroethylene substrate with the surface provided with the PS ball array by using the gas to obtain the polytetrafluoroethylene array. The specific experimental parameters were: the current is 3.2A, the pressure is 0.15Pa, the flow rate of sulfur hexafluoride gas is 35sccm, the power is 200w, and the etching time is 7 min.
(3) And sputtering a layer of copper film on the surface of the polytetrafluoroethylene array by using a magnetron sputtering method to obtain the copper array. The specific experimental parameters were: the vacuum degree is 30mTorr, the sputtering current is 40mA, the sputtering time is 5min, and the array with the surface covered with the copper film is obtained.
(4) And (3) soaking the copper array in a copper salt solution, and reacting to obtain the cuprous oxide array. First, 0.2000g of anhydrous copper sulfate (CuSO)4) Dissolved in 50mL of deionized water to obtain a copper sulfate solution. Soaking the array with the copper film covered on the surface in prepared copper sulfate solution for 15min, and thenAfter finishing reaction, taking out the substrate to obtain cuprous oxide array, alternately cleaning with deionized water and anhydrous ethanol for several times, and washing with N2And (5) standing after blow-drying.
(5) And (3) soaking the cuprous oxide array in a solution containing silver nitrate, and reacting to obtain the micro/nano structure array constructed by the silver nano sheets. Preparing a silver nitrate reaction solution: 0.0306g of silver nitrate, 0.0352g of anhydrous sodium citrate, and 10uL of concentrated nitric acid were dispersed in 20mL of deionized water, after which a 1cm × 1cm cuprous oxide substrate was placed in the mixed solution for 30 min. After the reaction is finished, taking out the substrate, alternately cleaning the substrate for a plurality of times by using deionized water and absolute ethyl alcohol, and using N2And drying to obtain the micro/nano structure array constructed by the silver nanosheets based on the polytetrafluoroethylene array.
Example 3
The method for converting any arbitrary nanocone array into a micro/nano-structure array constructed by silver nanosheets in situ, described in this embodiment 3, includes the following steps:
(1) and preparing a tightly arranged PS ball self-assembled single-layer film on the surface of the clean silicon substrate by using a gas-liquid interface self-assembly method. PS spheres with a diameter of 500nm were selected to obtain a tightly packed array of PS spheres monolayer on a 1cm by 1cm clean silicon substrate surface.
(2) Method of etching with reactive ions, using SF6And etching the silicon substrate with the PS ball array on the surface by using the gas to obtain the silicon array. The specific experimental parameters were: the current is 3A, the pressure is 0.1Pa, the flow rate of sulfur hexafluoride gas is 35sccm, the power is 200w, and the etching time is 3 min.
(3) And sputtering a layer of copper film on the surface of the silicon array by using a magnetron sputtering method to obtain the copper array. The specific experimental parameters were: the vacuum degree is 30mTorr, the sputtering current is 35mA, the sputtering time is 5min, and the array with the surface covered with the copper film is obtained.
(4) And (3) soaking the copper array in a copper salt solution, and reacting to obtain the cuprous oxide array. First, 0.2000g of anhydrous copper sulfate (CuSO)4) Dissolved in 50mL of deionized water to obtain a copper sulfate solution. Soaking the array with the copper film covered on the surface in a copper sulfate solution for 15minTaking out the substrate, alternately cleaning with deionized water and anhydrous ethanol for several times, and cleaning with N2And (5) standing after blow-drying to obtain the cuprous oxide array.
(5) And (3) soaking the cuprous oxide array in a solution containing silver nitrate, and reacting to obtain the micro/nano structure array constructed by the silver nano sheets. Preparing a silver nitrate reaction solution: 0.0153g of silver nitrate, 0.0176g of anhydrous sodium citrate, and 5uL of concentrated nitric acid were dispersed in 20mL of deionized water, after which a 1cm × 1cm cuprous oxide substrate was placed in the mixed solution for 15 min. After the reaction is finished, taking out the substrate, alternately cleaning the substrate for a plurality of times by using deionized water and absolute ethyl alcohol, and using N2And drying to obtain the micro/nano structure array constructed by the silver nano sheets based on the silicon array.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. A method for converting any nanocone array into a micro/nano structure array constructed by silver nanosheets in situ is characterized by comprising the following steps:
(1) preparing a single-layer film of PS balls which are arranged closely and self-assembled on the surface of a clean substrate by a gas-liquid interface self-assembly method;
(2) method of etching with reactive ions, using SF6Etching the substrate with the surface provided with the PS ball array by using gas to obtain any nano cone array structure;
(3) sputtering a layer of copper film on the surface of any nanocone array by using a magnetron sputtering method to obtain a copper array;
(4) soaking the copper array in a copper salt solution by utilizing a centering reaction between copper and the copper salt solution, and obtaining a cuprous oxide array after the reaction;
(5) soaking the cuprous oxide array in a solution containing silver nitrate, and reacting to obtain a micro/nano structure array constructed by silver nano sheets;
the step (1) comprises the following steps:
firstly, PS balls with the diameter of 120-1000 nm are selected, dispersed in deionized water and ethanol and subjected to ultrasonic treatment to be uniformly dispersed;
then, dropping PS balls on the surface of a clean glass slide with water added on the surface to form a single-layer film, drying for a period of time, transferring the glass slide to a beaker filled with water, wherein the single-layer film of the PS balls floats on the surface of the water, and fishing up the PS ball array on the surface of the water by utilizing a clean substrate of 1cm multiplied by 1cm, namely transferring the PS ball array to the surface of the substrate to obtain a closely-arranged PS ball single-layer film array, wherein the clean substrate is a silicon, glass, polytetrafluoroethylene or PE film;
the step (2) comprises the following steps:
and etching the substrate by taking the PS ball array as a mask, wherein the specific experimental parameters are as follows: the current is 0.5-5A, the pressure is 0.05-0.50 Pa, the flow rate of sulfur hexafluoride gas is 10-50 sccm, the power is 100-500 w, and the etching time is 30 s-9 min;
in the step (3), the specific experimental parameters are as follows:
the vacuum degree is 10-70 mTorr, the sputtering current is 15-90 mA, and the sputtering time is 2-30 min;
in the step (4), the copper salt includes copper nitrate, copper sulfate and/or copper acetate, and specifically includes:
preparing a copper salt solution: dissolving 0.0200-1.000 g of copper salt into 10-100 mL of deionized water to obtain a copper precursor solution;
then, soaking the nanocone array with the copper film covered on the surface in a precursor solution of copper, and setting the soaking time to be 10-30 min;
after the reaction is finished, taking out the substrate, and alternately cleaning the substrate for a plurality of times by using deionized water and absolute ethyl alcohol to obtain a cuprous oxide array;
with N2Drying to obtain a cuprous oxide array for the next reaction;
the step (5) comprises:
preparing a silver nitrate reaction solution: dispersing 0.0100-0.3000 g of silver nitrate, 0.0100-1.000 g of anhydrous sodium citrate and 5-50 uL of concentrated nitric acid into 5-50 mL of deionized water, and then placing a 1cm x 1cm cuprous oxide substrate in the mixed solution for soaking for 1-30 min;
after the reaction is finished, the substrate is taken out and is alternately cleaned for a plurality of times by deionized water and absolute ethyl alcohol.
2. The method for converting any nanocone array into a micro/nano structure array constructed by silver nanosheets in situ according to claim 1, wherein in step (1), the PS spheres have a size of 1000nm and the substrate is a silicon wafer.
3. The method for in-situ conversion of any nano-cone array into a micro/nano-structure array constructed by silver nano-sheets according to claim 1, wherein in the step (2), the current is 3A, the pressure is 0.1Pa, the flow rate of sulfur hexafluoride gas is 36sccm, the power is 200w, and the etching time is 7 min.
4. The method for converting any nanocone array into a micro/nano structure array constructed by silver nano sheets in situ according to claim 1, wherein in the step (3), the vacuum degree is 35mTorr, the sputtering current is 40mA, and the sputtering time is 5 min.
5. The method for in-situ conversion of arbitrary nanocone arrays into silver nanoplate-constructed micro/nanostructure arrays according to claim 1, wherein in the step (4), 0.4000g of anhydrous copper sulfate (CuSO)4) Dissolving into 50mL of deionized water to obtain a copper sulfate solution, and setting the soaking time to be 30 min.
6. The method for in-situ conversion of any nanocone array into a micro/nanostructure array constructed from silver nanoplates as in claim 1, wherein in step (5), 0.0306g of silver nitrate, 0.0352g of anhydrous sodium citrate, and 10uL of concentrated nitric acid are dispersed into 20mL of deionized water, after which 1cm x 1cm of cuprous oxide substrate is placed in the mixed solution for 30 min.
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