Preparation method of shuttlecock-shaped gold nanostructure

Abstract

The invention discloses a preparation method of a shuttlecock-shaped gold nanostructure, which comprises the following steps: firstly, carrying out ultrasonic and plasma cleaning on a silicon wafer, and simultaneously preparing a triaminopropyl trioxomethylsilane solution as a coupling agent; carrying out silanization treatment on the clean silicon wafer by using a coupling agent; preparing a gold nano seed growth solution from CTAC, chloroauric acid and sodium borohydride, and self-assembling gold nano seeds on the silicon wafer treated by the coupling agent; washing redundant gold nano seeds on the silicon wafer by using ultrapure water; preparing a secondary growth solution from CTAC, chloroauric acid, ascorbic acid and cysteine, and carrying out in-situ growth. The method for preparing the SERS structure is simple, economical and convenient, and the badminton-shaped gold nanostructure can be rapidly grown on the surface of the substrate in situ.

Description

Technical Field

[0001] The invention relates to a preparation technology of a gold nanostructure, in particular to a preparation method of a badminton-shaped gold nanostructure. Background Art

[0002] Since its discovery, surface-enhanced Raman scattering (SERS) has been extensively studied experimentally and theoretically to become one of the most sensitive spectroscopic tools due to its extremely high surface sensitivity and powerful application value in the qualitative and quantitative analysis of fingerprint vibrational spectra, even in SERS at the single-molecule level.

[0003] SERS has not developed into a robust surface technology as many had initially hoped, for one thing, only noble metals such as gold, silver and copper can provide large enhancement effects. Another thing is that even for these noble metals, surface roughness is critical to exhibit large enhancement factors.

[0004] In summary, the existing preparation technology has defects such as complicated steps and high process requirements.

[0005] In view of this, the present invention is proposed. Summary of the invention

[0006] The purpose of the present invention is to provide a method for preparing a badminton-shaped gold nanostructure to solve the above-mentioned technical problems existing in the prior art.

[0007] The objective of the present invention is achieved through the following technical solutions:

[0008] The method for preparing the badminton-shaped gold nanostructure of the present invention is characterized by comprising the following steps:

[0009] Step 1. First, the silicon wafer is cleaned by ultrasonic and plasma, and an APTMS solution is used as a coupling agent;

[0010] Step 2. Silanization treatment of the clean silicon wafer with a coupling agent;

[0011] Step 3. Prepare a gold nanoseed growth solution with CTAC, chloroauric acid and sodium borohydride, and self-assemble the gold nanoseeds on a silicon wafer treated with a coupling agent;

[0012] Step 4. Use ultrapure water to rinse the excess gold nanoseeds on the silicon wafer;

[0013] Step 5. Prepare the secondary growth solution with CTAC, chloroauric acid, ascorbic acid and cysteine ​​for in situ growth.

[0014] Compared with the prior art, the preparation method of the badminton-shaped gold nanostructure provided by the present invention uses a coupling agent to self-assemble gold nanoseeds on a substrate, and then uses a growth liquid to in-situ grow the badminton-shaped gold nanostructure at the seed. The preparation method meets the conditions of simplicity, economy, and flexibility, uses gold as the main material, and has a structure similar to a badminton. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 This is a field emission scanning electron microscope image of a typical badminton-shaped gold nanostructure prepared in an embodiment of the present invention;

[0016] Figure 2 For Figure 1 As a SERS substrate, the Raman spectra were measured in 4ATP solutions with concentrations ranging from 10-7 mol / L to 10-9 mol / L;

[0017] Figure 3 The figure is a flowchart of the steps of an embodiment of the present invention. DETAILED DESCRIPTION

[0018] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with the drawings in the embodiments of the present invention; it is obvious that the described embodiments are only part of the embodiments of the present invention, not all of the embodiments, which does not constitute a limitation of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the protection scope of the present invention.

[0019] First, the terms that may be used in this article are explained as follows:

[0020] The term “and / or” means that either or both of them can be realized at the same time. For example, X and / or Y means both “X” or “Y” and “X and Y”.

[0021] The terms "include", "comprises", "contains", "has" or other descriptions with similar semantics should be interpreted as non-exclusive inclusion. For example, including certain technical feature elements (such as raw materials, components, ingredients, carriers, dosage forms, materials, dimensions, parts, components, mechanisms, devices, steps, procedures, methods, reaction conditions, processing conditions, parameters, algorithms, signals, data, products or products, etc.) should be interpreted as including not only certain technical feature elements explicitly listed, but also other technical feature elements known in the art that are not explicitly listed.

[0022] The contents not described in detail in the examples of the present invention belong to the prior art known to professionals in the field. If no specific conditions are specified in the examples of the present invention, the conditions are carried out according to the conventional conditions in the field or the conditions recommended by the manufacturer. If the manufacturer is not specified in the reagents or instruments used in the examples of the present invention, they are all conventional products that can be purchased commercially.

[0023] The method for preparing the badminton-shaped gold nanostructure of the present invention comprises the following steps:

[0024] Step 1. First, the silicon wafer is cleaned by ultrasonic and plasma, and an APTMS solution is used as a coupling agent;

[0025] Step 2. Silanization treatment of the clean silicon wafer with a coupling agent;

[0026] Step 3. Prepare a gold nanoseed growth solution with CTAC, chloroauric acid and sodium borohydride, and self-assemble the gold nanoseeds on a silicon wafer treated with a coupling agent;

[0027] Step 4. Use ultrapure water to rinse the excess gold nanoseeds on the silicon wafer;

[0028] Step 5. Prepare the secondary growth solution with CTAC, chloroauric acid, ascorbic acid and cysteine ​​for in situ growth.

[0029] In step 1, methanol is used as a solvent for preparing an APTMS solution, and the concentration of the prepared APTMS solution is 10%.

[0030] In step 2, the temperature of the silanization treatment is 40° C., and the time of the silanization treatment is 2 h.

[0031] In step 3, the concentrations of CTAC, chloroauric acid, and sodium borohydride were 0.1 mol / L, 10 mmol / L, and 0.01 mol / L, respectively; the volumes of CTAC, chloroauric acid, and sodium borohydride were 5 mL, 0.125 mL, and 300 μL, respectively; and the growth time was 2 h.

[0032] In step 5, the concentrations of CTAC, chloroauric acid, ascorbic acid and cysteine ​​were 0.05 mol / L, 12.5 mmol / L, 0.05 mmol / L and 0.05 mol / L, respectively, the volumes of CTAC, chloroauric acid, ascorbic acid and cysteine ​​were 0.56 L, 80 μL, 100 μL and 950 μL, respectively, and the growth time was 2 h.

[0033] The prepared structure is a badminton-shaped gold nanostructure.

[0034] Also includes:

[0035] Step 6. Observe the silicon wafer substrate after the experiment under a scanning electron microscope to obtain a nanostructure image;

[0036] Step 7. Immerse the prepared sample in a tetraaminothiophenol (4-ATP) solution with a concentration of 10-7 mol / L to 10-9 mol / L to measure the Raman spectrum.

[0037] In summary, the method for preparing the badminton-shaped gold nanostructure of the embodiment of the present invention adopts an in-situ growth method to prepare the badminton-shaped gold nanostructure. First, a coupling agent is used to self-assemble gold nanoseeds on a substrate, and then the badminton-shaped gold nanostructure is grown in situ using this as a site. This method is simple, economical, and convenient for preparing a SERS structure, and can quickly grow a nanostructure in situ on the substrate surface.

[0038] The present invention proposes to use seeds to in-situ grow a badminton-shaped gold nanostructure on a substrate to prepare a SERS substrate. The method is simple, economical and convenient for preparing a SERS structure, can quickly grow a badminton-shaped gold nanostructure in-situ on the substrate surface, and can be used for trace detection of harmful molecules.

[0039] In order to more clearly demonstrate the technical solution and technical effects provided by the present invention, the embodiments of the present invention are described in detail with specific embodiments below.

[0040] Example 1

[0041] As shown in Figures 1 to 3, the embodiment provides a detailed introduction to the preparation steps of the badminton-shaped gold nanostructure, and the experimental supplies and equipment include: silicon wafer, APTMS, CTAC, chloroauric acid, sodium borohydride, ascorbic acid and cysteine, micro-area Raman spectrometer, ultrasonic cleaner, plasma cleaner, and ultrapure water machine.

[0042] The experimental steps are:

[0043] Step 1. First, the silicon wafer is cleaned by ultrasonic and plasma, and a 10% APTMS solution is prepared in methanol as a coupling agent.

[0044] Step 2. Silanize the clean silicon wafer with a coupling agent.

[0045] Step 3. Prepare the gold nanoseed growth solution with CTAC, chloroauric acid and sodium borohydride.

[0046] Step 4. Immerse the silicon wafer treated with the coupling agent to obtain self-assembled gold nanoseeds on the silicon wafer.

[0047] Step 5. Use ultrapure water to rinse the excess gold nanoseeds on the silicon wafer.

[0048] Step 6. Prepare a secondary growth solution with CTAC, chloroauric acid, ascorbic acid and cysteine ​​to in situ grow a badminton-shaped gold nanostructure.

[0049] Step 7. Observe the silicon wafer substrate after the experiment under a scanning electron microscope to obtain a nanostructure image, such as Figure 1 shown.

[0050] Step 8. Soak the prepared sample in a 4-ATP solution with a concentration of 10-7 mol / L to 10-9 mol / L and measure the Raman spectrum. Figure 2 shown.

[0051] In summary, Figure 1 This is a field emission scanning electron microscopy image of a typical badminton-shaped gold nanostructure prepared;

[0052] Figure 2 For Figure 1 Raman spectra measured in 4ATP solutions with concentrations ranging from 10-7 mol / L to 10-9 mol / L as SERS substrate;

[0053] Figure 3 It is a flow chart of the steps of the present invention.

[0054] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

[0055] The above is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily thought of by any technician familiar with the technical field within the technical scope disclosed in the present invention should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims. The information disclosed in the background technology section of this article is only intended to deepen the understanding of the overall background technology of the present invention, and should not be regarded as an admission or in any form that the information constitutes prior art known to those skilled in the art.

Claims

1. A method for preparing a badminton-shaped gold nanostructure, characterized in that: The steps include: Step 1. First, the silicon wafer is cleaned by ultrasonic and plasma, and an APTMS solution is used as a coupling agent; Step 2. Silanization treatment of the clean silicon wafer with a coupling agent; Step 3. Prepare a gold nanoseed growth solution with CTAC, chloroauric acid and sodium borohydride, and self-assemble the gold nanoseeds on a silicon wafer treated with a coupling agent; Step 4. Use ultrapure water to rinse the excess gold nanoseeds on the silicon wafer; Step 5. Prepare a secondary growth solution with CTAC, chloroauric acid, ascorbic acid and cysteine ​​for in situ growth.

2. The method for preparing a badminton-shaped gold nanostructure according to claim 1, characterized in that: In step 1, methanol was used as the solvent for preparing the APTMS solution.

3. The method for preparing a badminton-shaped gold nanostructure according to claim 2, characterized in that: In step 1, the concentration of the prepared APTMS solution is 10%.

4. The method for preparing a badminton-shaped gold nanostructure according to claim 1, characterized in that: In step 2, the temperature of the silanization treatment is 40° C., and the time of the silanization treatment is 2 h.

5. The method for preparing a badminton-shaped gold nanostructure according to claim 1, characterized in that: In step 3, the concentrations of CTAC, chloroauric acid, and sodium borohydride were 0.1 mol / L, 10 mmol / L, and 0.01 mol / L, respectively; the volumes of CTAC, chloroauric acid, and sodium borohydride were 5 mL, 0.125 mL, and 300 μL, respectively; and the growth time was 2 h.

6. The method for preparing a badminton-shaped gold nanostructure according to claim 1, characterized in that: In step 5, the concentrations of CTAC, chloroauric acid, ascorbic acid and cysteine ​​were 0.05 mol / L, 12.5 mmol / L, 0.05 mmol / L and 0.05 mol / L, respectively, the volumes of CTAC, chloroauric acid, ascorbic acid and cysteine ​​were 0.56 L, 80 μL, 100 μL and 950 μL, respectively, and the growth time was 2 h.

7. The method for preparing the badminton-shaped gold nanostructure according to any one of claims 1 to 6, characterized in that: The prepared structure is a badminton-shaped gold nanostructure.

8. The method for preparing a badminton-shaped gold nanostructure according to claim 7, characterized in that: Also includes: Step 6. Observe the silicon wafer substrate after the experiment under a scanning electron microscope to obtain a nanostructure image; Step 7. Immerse the prepared sample in a 4-ATP solution with a concentration of 10-7 mol / L to 10-9 mol / L to measure the Raman spectrum.

Images