CN111168079A - Method for synthesizing metal nanoparticles based on glass surface - Google Patents
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
- B22F2007/042—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
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- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/112—Deposition methods from solutions or suspensions by spraying
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
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Abstract
本发明公开了一种在基于玻璃表面合成金属纳米颗粒的方法，所述的方法为：向浓度为0.1mol·L‑1金属离子溶液加入浓度为0.15mol·L‑1的稀释剂溶液、低熔点玻璃粉、粘结剂，超声处理5‑10min后搅拌均匀，得到玻璃油墨混合物A喷涂在清洗干燥的玻璃基底上，控制喷涂厚度约为0.05～0.5mm，放置在干燥环境下烘干，干燥后利用紫外光辐照1h‑8h，辐照温度控制在140～160℃之间，将相应的金属离子还原生成对应的金属纳米颗粒，然后在保护性气氛下，在700‑800℃下热处理60‑120min，最后在保护性气氛保护下进行快速退火冷却处理，即得到表面覆盖金属纳米颗粒的玻璃基金属纳米材料。本发明制备工艺简单高效，制备周期短，且可操作性强，可以同时制备多种金属纳米颗粒及其复合材料。The invention discloses a method for synthesizing metal nanoparticles on a glass-based surface. The method comprises the following steps: adding a diluent solution with a concentration of 0.15mol·L -1 , a low The melting point glass powder and binder are ultrasonically treated for 5-10min and then stirred evenly to obtain glass ink mixture A, which is sprayed on the cleaned and dried glass substrate, and the spray thickness is controlled to be about 0.05-0.5mm, and placed in a dry environment for drying and drying After irradiating with ultraviolet light for 1h-8h, the irradiation temperature is controlled between 140-160°C, the corresponding metal ions are reduced to form corresponding metal nanoparticles, and then heat-treated at 700-800°C for 60 minutes in a protective atmosphere. ‑120min, and finally perform rapid annealing and cooling treatment under the protection of a protective atmosphere, that is, a glass-based metal nanomaterial whose surface is covered with metal nanoparticles is obtained. The preparation process of the invention is simple and efficient, the preparation period is short, and the operability is strong, and a variety of metal nanoparticles and their composite materials can be prepared simultaneously.
Description
Technical Field
The invention relates to a method for synthesizing metal nanoparticles based on a glass surface.
Background
Based on the excellent performance of the metal nano-particles and the unique performance of the metal nano-particles when the metal nano-particles are combined with other materials, the metal nano-particles have wide application prospect. The commonly used preparation methods of metal nanoparticles are: chemical reduction, laser ablation, electrochemistry, microwave irradiation and the like, wherein toxic reducing agents and stabilizing agents are used in the preparation methods, or toxic byproducts and the like are inevitably generated, so that potential environmental hidden dangers and biological application risks can be caused, the problems of low preparation efficiency, easy agglomeration in the product drying process, uncontrollable granularity and the like exist, in the practical application of the nano particles, the composition regulation and the stability of the nano particles are two problems troubling researchers, the composition and the size of the nano metal particles cannot be accurately regulated by a plurality of synthesis methods, and the phenomena of phase separation, agglomeration and the like easily occur in the subsequent heat treatment process, so that the method for preparing the metal nano particles simply, conveniently, efficiently and environmentally friendly is of great significance.
Disclosure of Invention
Aiming at the technical problem of preparing metal nanoparticles at the present stage, the invention provides a method for synthesizing metal nanoparticles based on glass surface, which is simple, convenient and efficient, has mild reaction conditions and controllable and stable size.
The technical scheme adopted by the invention is as follows:
a method for synthesizing metal nanoparticles based on a glass surface, comprising the steps of:
s1, 50-100 parts of the active carbon with the concentration of 0.1-0.5 mol.L-1Addition of metal ion solution20 to 100 parts of a solvent with a concentration of 0.1 to 0.5 mol/L-1Carrying out ultrasonic treatment on the diluent solution, 1-15 parts of low-melting-point glass powder and 1-10 parts of binder for 5-10min, and then uniformly stirring to obtain a glass ink mixture; the metal ion solution is Au-containing+、Ag+、Cu2+One or more of (a) and (b); s2, spraying the glass ink mixture obtained in the step S1 on a cleaned and dried glass substrate, controlling the spraying thickness to be about 0.05-0.5 mm, placing the glass substrate in a drying environment for drying, volatilizing organic components, and fixing metal ions;
s3, after drying, irradiating for 1-8 h by using ultraviolet light, controlling the irradiation temperature to be 140-160 ℃, reducing corresponding metal ions to generate corresponding metal nano particles, wherein the nano particles are slowly separated out and are basically spherical in shape;
s4, then carrying out heat treatment for 60-120min at 700-800 ℃ in a protective atmosphere, melting the low-melting-point glass powder, sintering the glass powder with a glass substrate, and uniformly fixing the generated nano particles on the glass substrate;
and S5, finally, carrying out rapid annealing cooling treatment under the protection of protective atmosphere to obtain the glass-based metal nano material with the surface covered with metal nano particles.
Further, the metal ion solution is HAuCl4Aqueous solution, AgNO3Aqueous solution or CuCl2An aqueous solution.
Further, in step S1, the diluent is one or more of PVP (polyvinylpyrrolidone), CTAB (cetyltrimethylammonium bromide) or PAM (polyacrylamide).
Further, in step S1, the melting point temperature of the low-melting-point glass frit is 450 to 700 ℃.
Further, in step S1, the binder is one or more of PVA, polyphosphoric acid (PPA), and sodium silicate.
Further, in step S2, the glass substrate is made of high temperature resistant and high light transmittance glass, and is cooled rapidly without breaking.
Further, in step S2, the drying condition is that the temperature is kept at 50-70 ℃ for 15-60min, the temperature is raised to 90-100 ℃ and kept for 20-80min, and then the mixture is naturally cooled to the room temperature.
Further, in step S3, the wavelength range of the ultraviolet light is preferably 190nm to 320 nm.
Further, in step S4, the protective atmosphere is nitrogen or argon.
Further, in step S5, the rapid annealing process: keeping the temperature at 300 ℃ for 15-60min, then heating to 450 ℃ and keeping the temperature for 10-60min, and then cooling to room temperature in protective atmosphere; the protective atmosphere is nitrogen or argon.
The particle size distribution of the metal nanoparticles of the glass-based metal nanoparticles obtained by the method is 10-500 nm.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation process is simple and efficient, the preparation period is short, the operability is strong, and various metal nano particles and composite materials thereof can be prepared simultaneously;
2. the uniform generation of the ion reduction reaction can be realized through the change of the illumination time and frequency, so that the granularity and the appearance of the product are controlled;
3. the preparation process is in a dry and tidy environment, the generation and protection of the particles are synchronously carried out, and the agglomeration of the nano particles is effectively prevented;
4. impurities are not introduced in the reaction, no by-product is generated, no excessive reagent pollutes the reaction product, and the obtained product has high purity and is convenient to collect;
5. after high-temperature heat treatment, the nano particles are fully combined with the glass substrate to obtain the novel glass-based material with the surface loaded with the metal nano particles, and the novel glass-based material can be used for catalyzing and degrading organic pollutants, photolyzing water, disinfecting and sterilizing and the like.
Detailed Description
The invention is further illustrated by the following specific examples:
the low-melting-point glass powder adopted by the invention is purchased from Ammi micro-nano, brand FR01 low-temperature glass state powder, the initial melting temperature is 430 ℃, PVP is PVP-K30 in Jiangyin Jiafeng chemical industry, and PVA is Shandong three-dimensional group 088-50.
Example 1
A method for synthesizing metal nano particles based on glass surface is characterized in that: the preparation method comprises the following steps:
s1, mixing 100ml of solution with the concentration of 0.1 mol.L-1HAuCl of4Adding 100ml of 0.15 mol.L into the solution-1Carrying out ultrasonic treatment on the PVP solution, 5g of low-melting-point glass powder and 5g of PVA for 5min, and then uniformly stirring to obtain a mixture A;
s2, spraying the mixture A on a cleaned and dried glass substrate, controlling the spraying thickness to be about 0.05mm, placing the glass substrate in a drying environment for drying, keeping the temperature of 70 ℃ for 20min under the drying condition, heating to 100 ℃ for 30min, and naturally cooling to room temperature;
s3, after drying, irradiating for 4 hours by using ultraviolet light of 260-320nm, and reducing corresponding metal ions to generate corresponding Au nano-particles;
s4, carrying out high-temperature heat treatment at 700 ℃ for 60min under the nitrogen atmosphere, and uniformly fixing the generated nano particles on a glass substrate;
s5, finally, carrying out rapid annealing cooling treatment under the protection of nitrogen atmosphere, preserving heat for 15min at 300 ℃, then heating to 450 ℃, preserving heat for 20min, and cooling to room temperature to obtain the novel glass-based metal nano material with the surface covered with the Au nano particles, and representing the generated nano particles by using an ultraviolet-visible spectrum, wherein a spectrum curve can show a characteristic peak of the spherical gold nano particles, the wavelength of lambda max is stable and is about 520.0nm, and the peak shape is stable, so that the more uniform spherical gold nano particles can be obtained under the experimental conditions.
Example 2
A method for synthesizing metal nano particles based on glass surface is characterized in that: the preparation method comprises the following steps:
s1, mixing 100ml of solution with the concentration of 0.1 mol.L-1AgNO of3Adding 100ml of 0.15 mol.L into the solution-1Carrying out ultrasonic treatment on the PVP solution, 5g of low-melting-point glass powder and 5g of PVA for 5min, and then uniformly stirring to obtain a mixture A;
s2, spraying the mixture A on a cleaned and dried glass substrate, controlling the spraying thickness to be about 0.1mm, placing the glass substrate in a drying environment for drying, keeping the temperature of 70 ℃ for 20min under the drying condition, heating to 100 ℃ for 30min, and naturally cooling to room temperature;
s3, after drying, irradiating for 4 hours by using ultraviolet light with the wavelength of 190-260nm, and reducing corresponding metal ions to generate corresponding Ag nano particles;
s4, then carrying out high-temperature heat treatment at 700 ℃ for 60 min;
s5, finally, carrying out rapid annealing cooling treatment under the protection of nitrogen atmosphere, preserving heat for 15min at 300 ℃, then heating to 450 ℃, preserving heat for 20min, and cooling to room temperature to obtain the novel glass-based metal nano material with the surface covered with Ag nano particles, and representing the generated nano particles by using an ultraviolet-visible spectrum, wherein a spectrum curve can be found to present a characteristic peak of the spherical silver nano particles, the wavelength of lambda max is stable and is about 410.0nm, and the peak shape is stable, so that more uniform spherical silver nano particles can be obtained under the experimental conditions.
Example 3, a method for synthesizing metal nanoparticles based on a glass surface, characterized in that: the preparation method comprises the following steps:
s1, mixing 100ml of solution with the concentration of 0.1 mol.L-1CuCl of2Adding 100ml of 0.15 mol.L into the solution-1Carrying out ultrasonic treatment on the PVP solution, 5g of low-melting-point glass powder and 5g of PVA for 5min, and then uniformly stirring to obtain a mixture A;
s2, spraying the mixture A on a cleaned and dried glass substrate, controlling the spraying thickness to be about 0.5mm, placing the glass substrate in a drying environment for drying, keeping the temperature of 70 ℃ for 20min under the drying condition, heating to 100 ℃ for 30min, and naturally cooling to room temperature;
s3, after drying, irradiating for 4 hours by using 190-320nm ultraviolet light, and reducing corresponding metal ions to generate corresponding Cu nano particles;
s4, then carrying out high-temperature heat treatment at 700 ℃ for 60min in a nitrogen atmosphere;
s5, finally, carrying out rapid annealing cooling treatment under the protection of nitrogen atmosphere, preserving heat for 15min at 300 ℃, then heating to 450 ℃, preserving heat for 20min, and cooling to room temperature to obtain the novel glass-based metal nano material with the surface covered with the Cu nano particles, and characterizing the generated nano particles by using an ultraviolet-visible spectrum, wherein a spectrum curve shows a characteristic peak of the spherical copper nano particles, the wavelength of the lambda max is stable and is about 500.0nm, and the peak shape is stable, so that the more uniform spherical silver nano particles can be obtained under the experimental conditions.
Although the present invention has been described with reference to preferred embodiments, it will be understood by those skilled in the art that the present invention may be practiced without limitation to the foregoing embodiments and within the scope of the appended claims.
Claims (10)
1. A method for synthesizing metal nano particles based on glass surface is characterized in that: the method comprises the following steps:
s1, 50-100 parts of the active carbon with the concentration of 0.1-0.5 mol.L-1Adding 20-100 parts of metal ion solution with the concentration of 0.1-0.5 mol.L-1Carrying out ultrasonic treatment on the diluent solution, 1-15 parts of low-melting-point glass powder and 1-10 parts of binder for 5-10min, and then uniformly stirring to obtain a glass ink mixture A; the metal ion solution is Au-containing+、Ag+、Cu2+One or more of (a) and (b);
s2, spraying the mixture A obtained in the step S1 on a cleaned and dried glass substrate, controlling the spraying thickness to be about 0.05-0.5 mm, and placing the glass substrate in a drying environment for drying;
s3, after drying, irradiating for 1-8 h by using ultraviolet light, controlling the irradiation temperature to be 140-160 ℃, and reducing corresponding metal ions to generate corresponding metal nano-particles;
s4, then carrying out heat treatment for 60-120min at 700-800 ℃ in a protective atmosphere, and uniformly fixing the generated nano particles on a glass substrate;
and S5, finally, carrying out rapid annealing cooling treatment under the protection of protective atmosphere to obtain the glass-based metal nano material with the surface covered with metal nano particles.
2. The method of claim 1, wherein: the metal ion solution is HAuCl4Aqueous solution, AgNO3Aqueous solution or CuCl2An aqueous solution.
3. The method of claim 1, wherein: in step S1, the diluent is one or more of polyvinylpyrrolidone, cetyltrimethylammonium bromide, and polyacrylamide.
4. The method of claim 1, wherein: in step S1, the melting point temperature of the low-melting-point glass powder is 450-700 ℃.
5. The method of claim 1, wherein: in step S1, the binder is one or more of PVA, polyphosphoric acid, or sodium silicate.
6. The method of claim 1, wherein: in step S2, the glass substrate is made of high temperature resistant and high light transmittance glass, and is cooled rapidly without breaking.
7. The method of claim 1, wherein: in step S2, the drying condition is that the temperature is kept at 50-70 ℃ for 15-60min, the temperature is raised to 90-100 ℃ and kept for 20-80min, and then the temperature is naturally cooled to the room temperature.
8. The method of claim 1, wherein: in step S3, the wavelength range of the ultraviolet light is 190nm to 320 nm.
9. The method of claim 1, wherein: in step S4, the protective atmosphere is nitrogen or argon.
10. The method of claim 1, wherein: in step S5, the rapid annealing process: keeping the temperature at 300 ℃ for 15-60min, then heating to 450 ℃ and keeping the temperature for 10-60min, and then cooling to room temperature in protective atmosphere; the protective atmosphere is nitrogen or argon.
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