CN111168079B - Method for synthesizing metal nanoparticles based on glass surface - Google Patents
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- CN111168079B CN111168079B CN202010041792.2A CN202010041792A CN111168079B CN 111168079 B CN111168079 B CN 111168079B CN 202010041792 A CN202010041792 A CN 202010041792A CN 111168079 B CN111168079 B CN 111168079B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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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- 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
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/112—Deposition methods from solutions or suspensions by spraying
-
- 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
- C03C2218/32—After-treatment
Abstract
The invention discloses a method for synthesizing metal nano particles on the surface of glass, which comprises the following steps: to a concentration of 0.1 mol. L ‑1 The metal ion solution is added with the concentration of 0.15 mol.L ‑1 The diluent solution, the low-melting-point glass powder and the binder are subjected to ultrasonic treatment for 5-10min and then uniformly stirred to obtain a glass ink mixture A, the glass ink mixture A is sprayed on a cleaned and dried glass substrate, the spraying thickness is controlled to be about 0.05-0.5 mm, the glass ink mixture A is placed in a drying environment and dried, then the glass ink mixture A is irradiated for 1-8 h by ultraviolet light after being dried, the irradiation temperature is controlled to be 140-160 ℃, corresponding metal ions are reduced to generate corresponding metal nano particles, then the heat treatment is carried out for 60-120min at 700-800 ℃ under the protective atmosphere, and finally the rapid annealing cooling treatment is carried out under the protective atmosphere, so that the glass base metal nano material with the surface covered with the metal nano particles is obtained. The preparation method has the advantages of simple and efficient preparation process, short preparation period and strong operability, and can be used for simultaneously preparing various metal nano particles and composite materials thereof.
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 to 100 portions of the product with the concentration of 0.1 to 0.5 mol.L -1 Adding 20-100 parts of metal ion solution with the concentration of 0.1-0.5 mol.L -1 The diluent solution, 1-15 parts of low-melting-point glass powder and 1-10 parts of binder are subjected to ultrasonic treatment for 5-10min and then are uniformly stirred to obtain a glass ink mixture; the metal ion solution is Au-containing + 、Ag + 、Cu 2+ 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 together, 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 the metal nano particles.
Further, the metal ion solution is HAuCl 4 Aqueous solution, agNO 3 Aqueous solution or CuCl 2 An aqueous solution.
Further, in step S1, the diluent is one or more of PVP (polyvinylpyrrolidone), CTAB (cetyltrimethylammonium bromide) or PAM (polyacrylamide).
Further, in the step S1, the melting point temperature of the low-melting-point glass powder is 450-700 ℃.
Further, in step S1, the binder is one or more of PVA, polyphosphoric acid (PPA) or sodium silicate.
Further, in the step S2, the glass substrate is made of high-temperature-resistant and high-transmittance glass, and is rapidly cooled without breaking.
Further, in step S2, the drying condition is that the temperature is kept for 15-60min at 50-70 ℃, the temperature is raised to 90-100 ℃, the temperature is 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 320nm.
Further, in step S4, the protective atmosphere is nitrogen or argon.
Further, in step S5, the rapid annealing treatment: 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 metal nanoparticles of the glass-based metal nanoparticles obtained by the present invention have a particle size distribution of 10 to 500nm.
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 Jiangyin Jia Feng Huagong PVP-K30, 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 -1 HAuCl of 4 Adding 100ml of 0.15 mol.L into the solution -1 Carrying 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 -1 AgNO of 3 Adding 100ml of 0.15 mol.L into the solution -1 Carrying 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 60min;
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, 100ml of the solution with the concentration of 0.1 mol.L -1 CuCl of 2 Adding 100ml of 0.15 mol.L into the solution -1 Carrying 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, drying the glass substrate in the drying environment, keeping the temperature of 70 ℃ for 20min, heating the glass substrate to 100 ℃, keeping the temperature for 30min, and naturally cooling the glass substrate 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 (9)
1. A method for synthesizing metal nano particles based on glass surface is characterized in that: the method comprises the following steps:
s1, 50 to 100 portions of the product with the concentration of 0.1 to 0.5 mol.L -1 Adding 20-100 parts of metal ion solution with the concentration of 0.1-0.5 mol.L -1 The diluent solution, 1-15 parts of low-melting-point glass powder and 1-10 parts of binder are subjected to ultrasonic treatment for 5-10min and then are uniformly stirred to obtain a glass ink mixture A; the metal ion solution is Au-containing + 、Ag + 、Cu 2+ One or more of (a) and (b); the melting point temperature of the low-melting-point glass powder is 450-700 DEG C；
S2, spraying the mixture A obtained in the step S1 on a cleaned and dried glass substrate, controlling the spraying thickness to be 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, carrying out heat treatment at 700-800 ℃ for 60-120min under a protective atmosphere to generate nano particles which are uniformly fixed 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 HAuCl 4 Aqueous solution, agNO 3 Aqueous solution or CuCl 2 An aqueous solution.
3. The method of claim 1, wherein: in the step S1, the diluent is one or a mixture of polyvinyl pyrrolidone, cetyl trimethyl ammonium bromide or polyacrylamide.
4. The method of claim 1, wherein: in the step S1, the binder is one or a mixture of PVA, polyphosphoric acid or sodium silicate.
5. The method of claim 1, wherein: in the step S2, the glass substrate is made of high-temperature-resistant high-light-transmittance glass, and is rapidly cooled without cracking.
6. The method of claim 1, wherein: in the step S2, the drying condition is that the temperature is kept for 15-60min at 50-70 ℃, the temperature is increased to 90-100 ℃, the temperature is kept for 20-80min, and then the mixture is naturally cooled to the room temperature.
7. The method of claim 1, wherein: in step S3, the wavelength range of the ultraviolet light is 190nm-320nm.
8. The method of claim 1, wherein: in step S4, the protective atmosphere is nitrogen or argon.
9. The method of claim 1, wherein: in step S5, the rapid annealing cooling treatment: 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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