Method for regulating and controlling growth of particles on surface of silver alloy membrane through freezing
By freezing the silver alloy film, the growth of silver particles is regulated, and the complex operation, high cost and environmental protection problems in the existing technology are solved, and the silver particles are small in size and uniformly distributed, improving the growth control effect.
Patent Information
- Application Number
- CN202510009776.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-03
- Publication Date
- 2025-04-11
AI Technical Summary
In the prior art, when preparing silver nanoparticles, a variety of chemical reagents are often used. The operation is complex, the products are prone to agglomeration, and the sizes are different. There is a potential risk to the human body and the environment, and the physical method consumes energy and costs high.
By freezing the silver alloy film, the atomic diffusion behavior of the silver alloy film is regulated, the silver atoms are hindered from diffusion along the normal direction, and the further growth of silver particles is inhibited, and the silver particles are formed smaller in size and more uniformly distributed.
The silver particles are smaller in size and more uniform in distribution, simplified operation, reduced costs, and environmentally friendly, improving the growth control effect of silver particles on the surface of the silver alloy film.
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Figure CN119800308A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of silver alloy films, in particular to a method for freezing and regulating the growth of particles on the surface of a silver alloy film. Background Art
[0002] In recent years, silver nanoparticles (Ag NPs) have attracted extensive attention in the fields of photocatalysis, ultrasensitive chemistry, biosensors, etc. due to their significant surface and interface effects, unique quantum size effects, and excellent localized surface plasmon resonance effects. In particular, their localized surface plasmon resonance effects, which are superior to those of precious metals such as gold and copper, have become an important material for preparing surface enhanced Raman scattering (SERS) substrates and improving the sensitivity of modern detection technologies. In addition, with the abuse of antibiotics in the development and use of a large number of new pharmaceutical products, the resistance of microorganisms and viruses to antibiotics has gradually become a global problem. As inorganic antibacterial agents, silver nanomaterials have become the key to solving the problem of antibiotic resistance with their broad-spectrum antibacterial properties, no resistance, and low toxicity. Studies have shown that the performance of silver nanomaterials depends on their size, composition, and shape. Therefore, how to obtain Ag NPs with uniform size, uniform distribution, and not easy to agglomerate has become the key to obtaining materials with good SERS performance and antibacterial properties.
[0003] At present, researchers usually use various biological, chemical and physical methods to prepare Ag NPs, such as chemical reduction, photochemical reduction, electrochemical reduction and biological reduction. Ag salts are reduced by using various chemical reductants or biological reductants, and the shape and size of Ag NPs are controlled by using end-capping agents such as citrate, chitosan, carboxymethyl cellulose (CMC), 1-dodecyl mercaptan (DDT) and polyvinyl pyrrolidone (PVP). However, this type of preparation method often involves the use of multiple chemical reagents. Not only is the operation process complicated, the prepared particles are easy to agglomerate and have different sizes, and there are potential risks to the human body and the environment during use. Physical methods generally use high temperature or high pressure, such as laser ablation, which consumes energy and is costly.
[0004] Therefore, it is necessary to explore a green, simple, and low-cost method to obtain AgNPs with fine particles and uniform distribution. Summary of the invention
[0005] In order to address the deficiencies in the prior art, the present invention provides a method for freezing and regulating the growth of particles on the surface of a silver alloy film. By freezing the silver alloy film, the atomic diffusion behavior of the silver alloy film can be regulated, causing the self-formed silver particles on the surface of the silver alloy film to be smaller in size and more evenly distributed.
[0006] In order to achieve the above object, the specific scheme adopted by the present invention is: A method for freezing and regulating the growth of particles on the surface of a silver alloy film, mainly comprising the following steps: Step S1, magnetron sputtering a silver alloy film on the surface of the flexible substrate; Step S2, placing the flexible substrate sputtered with the silver alloy film in a container filled with water, submerging the flexible substrate in the water, and placing the container in a freezer for freezing treatment for 1-7 days; Step S3: After freezing, take out, thaw and dry.
[0007] Furthermore, in step S1, the silver alloy film is an Ag-Nb alloy film or an Ag-W alloy film.
[0008] Furthermore, the silver alloy film is an Ag-(25-40)%Nb alloy film.
[0009] Furthermore, in step S1, the thickness of the silver alloy film is 50 nm.
[0010] Furthermore, in step S1, the material of the flexible substrate is polyimide.
[0011] Furthermore, in step S2, the temperature of the freezing treatment is -18°C.
[0012] Beneficial effects:
[0013] (1) The present invention regulates the atomic diffusion behavior of the silver alloy film by freezing the silver alloy film on the flexible substrate. During the freezing process, the silver alloy film is frozen in the middle of the ice layer. The ice layer and the silver alloy film are tightly attached to each other, which can hinder the diffusion of atoms on the surface of the silver alloy film along the normal direction and reduce the diffusion distance of Ag atoms, thereby inhibiting the further growth of the self-grown particles on the surface of the silver alloy film, and promoting the self-formation of silver particles with smaller size and more uniform distribution on the surface of the silver alloy film.
[0014] (2) The method of the present invention is simple, easy to operate, low in cost, and environmentally friendly. It can effectively regulate the growth of silver particles on the surface of the silver alloy film and obtain a large specific surface area Ag particle / alloy film with uniform structure on a flexible substrate. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] Figure 1 This is the organizational diagram of the product prepared in Example 1.
[0016] Figure 2 This is the organizational diagram of the product prepared in Example 2.
[0017] Figure 3 This is the organizational diagram of the product prepared in Example 3.
[0018] Figure 4This is the organizational diagram of the product prepared in Comparative Example 1.
[0019] Figure 5 This is the organizational diagram of the product prepared for Comparative Example 2.
[0020] Figure 6 This is the organizational diagram of the product prepared for Comparative Example 3. DETAILED DESCRIPTION
[0021] The present invention discloses a method for freezing and regulating the growth of particles on the surface of a silver alloy film, which is characterized by mainly comprising the following steps: Step S1, magnetron sputtering a 50 nm thick silver alloy film on the surface of the flexible substrate; Step S2, placing a flexible substrate (such as a polyimide substrate) sputtered with a silver alloy film in a container filled with water, submerging the flexible substrate in water, and placing the container in a freezer at -18°C for freezing for 1-7 days; inserting the flexible substrate Ag alloy film into a plastic box filled with water, and then placing the plastic box in the freezer for freezing for 1-7 days. During the freezing process, the Ag alloy film is completely wrapped by ice, and the ice layer tightly covers the surface of the Ag alloy film, which can hinder the diffusion of atoms on the surface of the alloy film in the normal direction, thereby inhibiting the further growth of particles self-grown on the surface of the alloy film, and promoting the self-formed particles on the surface of the Ag alloy film to be smaller in size and more evenly distributed; Step S3: After freezing, take out the sample, thaw it and dry it.
[0022] It should be noted that in step S1, the silver alloy film is an Ag-(25-40)% Nb alloy film or an Ag-W alloy film.
[0023] The technical solution of the present invention will be clearly and completely described below in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.
[0024] Example 1
[0025] The present invention discloses a method for freezing and regulating the growth of particles on the surface of a silver alloy film, which is characterized by mainly comprising the following steps: Step S1, preparing a 50 nm thick Ag-25% Nb alloy film on a polyimide substrate (substrate size is 30 mm long, 7 mm wide, substrate thickness is 0.125 mm) by magnetron sputtering method; Step S2, inserting the polyimide substrate sputtered with the silver alloy film into a plastic box filled with water, and then putting the plastic box into a freezer at -18°C for 1 day; Step S3: After freezing, take out the sample, thaw it and dry it.
[0026] Example 2
[0027] The present invention discloses a method for freezing and regulating the growth of particles on the surface of a silver alloy film, which is characterized by mainly comprising the following steps: Step S1, preparing a 50 nm thick Ag-32.7% Nb alloy film on a polyimide substrate (substrate size is 30 mm long, 7 mm wide, and substrate thickness is 0.125 mm) by magnetron sputtering method; Step S2, inserting the polyimide substrate sputtered with the silver alloy film into a plastic box filled with water, and then putting the plastic box into a freezer at -18°C for 3 days; Step S3: After freezing, take out the sample, thaw it and dry it.
[0028] Example 3
[0029] The present invention discloses a method for freezing and regulating the growth of particles on the surface of a silver alloy film, which is characterized by mainly comprising the following steps: Step S1, preparing a 50 nm thick Ag-40% Nb alloy film on a polyimide substrate (substrate size is 30 mm long, 7 mm wide, substrate thickness is 0.125 mm) by magnetron sputtering method; Step S2, inserting the polyimide substrate sputtered with the silver alloy film into a plastic box filled with water, and then putting the plastic box into a freezer at -18°C for 7 days; Step S3: After freezing, take out the sample, thaw it and dry it.
[0030] Comparative Example 1
[0031] The difference between Comparative Example 1 and Example 1 is that: Step S2, inserting the polyimide substrate sputtered with the silver alloy film into a plastic box filled with water, placing it at room temperature, and naturally curing it for 1 day.
[0032] Comparative Example 2
[0033] The difference between Comparative Example 2 and Example 2 is that: Step S2, inserting the polyimide substrate sputtered with the silver alloy film into a plastic box filled with water, placing it at room temperature, and naturally curing it for 3 days.
[0034] Comparative Example 3
[0035] The difference between Comparative Example 3 and Example 3 is that: Step S2, inserting the polyimide substrate sputtered with the silver alloy film into a plastic box filled with water, placing it at room temperature, and naturally curing it for 7 days.
[0036] Figure 1-6The organizational diagrams of the products prepared in Examples 1-3 and Comparative Examples 1-3 are shown in Table 1. The average number and average size of silver particles per unit area (1 mm*1 mm) are calculated based on the organizational diagrams.
[0037] Table 1 Average number and average size of silver particles per unit area Average number of silver particles per unit area Average size of silver particles per unit area (nm) Example 1 52 38 Example 2 69 32 Example 3 130 36 Comparative Example 1 21 45 Comparative Example 2 44 52 Comparative Example 3 60 67
[0038] As shown in Table 1, compared with the sample without freezing treatment in Comparative Example 1, the number of silver particles formed per unit area of the sample after freezing treatment in Example 1 increased by 148%, and the average particle size decreased by 16%. Compared with the sample without freezing treatment in Comparative Example 2, the number of silver particles formed per unit area of the sample after freezing treatment in Example 2 increased by 57%, and the average particle size decreased by 38%. Compared with the sample without freezing treatment in Comparative Example 3, the number of silver particles formed per unit area of the sample after freezing treatment in Example 3 increased by 117%, and the average particle size decreased by 46%. It can be seen that the present invention does achieve the effect of regulating the growth of silver particles on the surface of the silver alloy film through freezing treatment.
[0039] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Any equivalent changes or modifications made according to the essence of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for freezing and regulating the growth of particles on the surface of a silver alloy film, characterized in that: The main steps are as follows: Step S1, magnetron sputtering a silver alloy film on the surface of the flexible substrate; Step S2, placing the flexible substrate sputtered with the silver alloy film in a container filled with water, submerging the flexible substrate in the water, and placing the container in a freezer for freezing treatment for 1-7 days; Step S3: After freezing, take out, thaw and dry.
2. The method for freezing and regulating the growth of particles on the surface of a silver alloy film according to claim 1, characterized in that: In step S1, the silver alloy film is an Ag-Nb alloy film or an Ag-W alloy film.
3. The method for freezing and regulating the growth of particles on the surface of a silver alloy film according to claim 2, characterized in that: The silver alloy film is an Ag-(25-40)% Nb alloy film.
4. The method for freezing and regulating the growth of particles on the surface of a silver alloy film according to claim 1, characterized in that: In step S1, the thickness of the silver alloy film is 50 nm.
5. The method for freezing and regulating the growth of particles on the surface of a silver alloy film according to claim 1, characterized in that: In step S1 , the material of the flexible substrate is polyimide.
6. The method for freezing and regulating the growth of particles on the surface of a silver alloy film according to claim 1, characterized in that: In step S2, the temperature of the freezing treatment is -18°C.