CN113149429B - High borosilicate glass containing metal nanoparticles and preparation method thereof - Google Patents
High borosilicate glass containing metal nanoparticles and preparation method thereof Download PDFInfo
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/102—Glass compositions containing silica with 40% to 90% silica, by weight containing lead
- C03C3/105—Glass compositions containing silica with 40% to 90% silica, by weight containing lead containing aluminium
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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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
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Abstract
The invention provides a high-efficiency, simple and stable-performance method for synthesizing high borosilicate glass containing metal nano particles. Mixing the following components in percentage by mass: 940-997 parts of high borosilicate glass batch, 0.2-10 parts of metal compound micro powder with the grain diameter of 200-1600 meshes and 2-50 parts of reducing agent to obtain a premix; carrying out melt heat treatment on the premix at 1450-1800 ℃ for 1-4h under a protective atmosphere A, annealing at 400-550 ℃ for 30-90 min, and cooling to room temperature; irradiating the glass containing the metal ions by X-rays at room temperature for 30-120 min, then carrying out heat treatment at 400-700 ℃ for 30-90 min under the protective atmosphere B, and cooling to room temperature to obtain the high borosilicate glass containing the metal nanoparticles. The invention can prepare the high borosilicate glass composite material containing metal nano particles with good stability.
Description
(I) technical field
The invention relates to a high borosilicate glass composite material containing metal nano particles and a preparation method thereof.
(II) background of the invention
Metal nanoparticles (e.g., au, ag, cu, etc.) are of particular interest because of their unique surface plasmon resonance effects, quantum size effects, and localized field effects. The metal nano-particles are introduced into the glass matrix, and the local field intensity is increased due to the excitation of surface plasmon of the metal nano-particles, so that the metal nano-particles can generate better nonlinear optical properties and have wide application prospects in the field of optical devices with specific optical functions.
Researches find that the nonlinear optical properties of the material are greatly influenced by the size, the particle size distribution, the crystallization degree and the like of metal nanoparticles, and the type of the glass matrix also has a large influence on the material. At present, the glass substrate is generally selected from common soda-lime silicate series glass with poor optical, thermal and mechanical properties, and the effect and the application range of the material are limited. The high borosilicate glass has excellent properties (such as good transparency, low glass transition temperature (Tg), high density, high thermal expansion coefficient (easy to manufacture optical fiber), suitable bandwidth, good infrared transmittance, etc.), and is more suitable as a matrix of a glass material containing metal nanoparticles. Common methods for generating metal nanoparticles in traditional soda-lime-silica glass with a loose network structure include an ion implantation method, an ion exchange method, a sol-gel method, a fusion heat treatment method and the like, but because the network structure of high borosilicate glass is compact, the nanoparticles synthesized by the traditional process have poor uniformity and poor stability and controllability.
In view of the above problems, it is important to develop a method for preparing nano metal particles with good uniformity and stability in high borosilicate glass.
Disclosure of the invention
Aiming at the problems in the prior art, the invention provides a high-efficiency, simple and convenient method for synthesizing high borosilicate glass containing metal nano particles with stable performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of high borosilicate glass containing metal nano particles, which comprises the following steps:
(1) Mixing the following components in parts by mass: 940-997 parts (preferably 975-994 parts) of high borosilicate glass batch, 0.2-10 parts (preferably 0.8-5 parts) of metal compound micro powder with the particle size of 200-1600 meshes and 2-50 parts (preferably 5-20 parts) of reducing agent to obtain a premix; the metal compound of the metal compound micro powder is AgNO 3 、HAuCl 4 ·4H 2 O、Cu 2 One or more of O; the reducing agent is SnO or Sb 2 O 5 、CeO 2 One or more of (a); the high borosilicate glass batch is composed of the following components in parts by mass: 780-850 parts of silicon dioxide (SiO) 2 ) 170 to 270 portions of boric acid (H) 3 BO 3 ) 68-172 parts of sodium carbonate (Na) 2 CO 3 ) 0 to 76 parts of aluminum hydroxide (Al (OH) 3 ) And 0-90 parts of calcium carbonate (CaCO) 3 )；
(2) Melting and heat-treating the premix obtained in the step (1) at 1450-1800 ℃ for 1-4 h under a protective atmosphere A, injecting the obtained glass melt into a mold, annealing at 400-550 ℃ for 30-90 min, and cooling to room temperature to obtain glass containing metal ions;
(3) And (3) irradiating the glass containing the metal ions in the step (2) by X-ray at room temperature (CuK alpha, lambda =0.15416nm,50kV and 50mA) for 30-120 min, then carrying out heat treatment at 400-700 ℃ in a protective atmosphere B for 30-90 min, and cooling to obtain the high borosilicate glass containing the metal nanoparticles.
Preferably, the high borosilicate glass batch material in the step (1) has the composition of 788 parts of silicon dioxide (SiO) 2 ) 226 parts of boric acid (H) 3 BO 3 ) 97 portions of sodium carbonate (Na) 2 CO 3 ) 30 parts of aluminum hydroxide (Al (OH) 3 ) 5 parts of calcium carbonate (CaCO) 3 )。
Preferably, the metal compound of the metal compound micropowder in the step (1) is AgNO 3 、Cu 2 One or two of O, and AgNO is especially preferable 3 。
Preferably, the reducing agent in the step (1) is SnO or CeO 2 One or two of them.
Preferably, the protective atmosphere A in the step (2) or the protective atmosphere B in the step (3) is a nitrogen or argon atmosphere.
Preferably, the temperature of the melting heat treatment in the step (2) is 1500-1750 ℃ and the time is 1-2 h.
Preferably, the X-ray irradiation time of the glass powder containing metal ions in the step (3) is 30-60 min, and the glass powder is subjected to heat treatment at 500-600 ℃ for 30-60 min under the protective atmosphere B.
Compared with the prior art, the invention has the beneficial effects that: the high borosilicate glass composite material containing metal nano particles with good stability can be prepared, the preparation process is efficient and simple, and the high borosilicate glass composite material is suitable for preparing various metal nano particles.
(IV) description of the drawings
FIG. 1 shows the content of AgNO 0.08% 3 And 1.5% SnO by optical absorption Spectroscopy of high borosilicate glass annealed at 400 ℃ for 60min after X-ray irradiation.
FIG. 2 represents the content of AgNO 0.15% 3 And 1.0% SnO by optical absorption spectrum annealed at 600 ℃ for 60min after X-ray irradiation.
FIG. 3 represents the content of AgNO 0.08% 3 And 1.5% SnO by weight, optical absorption spectrum of high borosilicate glass annealed at 600 ℃ for 60min after X-ray irradiation.
FIG. 4 shows a composition containing Ag + The common glass is annealed for 60min at 420 ℃ and 560 ℃ respectively after being irradiated by X-rays.
(V) detailed description of the preferred embodiments
The present invention is further illustrated by the following specific examples, but the scope of the invention is not limited thereto. The borosilicate glass batch materials selected for use in the following examples were introduced into each group by selecting reagent grade SiO 2 、H 3 BO 3 、Na 2 CO 3 、Al(OH) 3 And CaCO 3 Weighing 788g of SiO 2 、226g H 3 BO 3 、97g Na 2 CO 3 、30g Al(OH) 3 And 5g of CaCO 3 And uniformly mixing to obtain the high borosilicate glass batch. The theoretical mass composition (wt%) of the high borosilicate glass is SiO 2 :78.8；B 2 O 3 :12.8；Na 2 O:5.7；Al 2 O 3 :2.0；CaO:0.3。
Example 1:
a method for synthesizing metal nanoparticles in high borosilicate glass, characterized by: the preparation method comprises the following steps:
(1) 98.42g of a high borosilicate glass batch with 0.1259g of AgNO 3 Then adding 1.7g of SnO reducing agent, mixing in equal proportion, and grinding and mixing in a ceramic mortar for 30min to obtain 99.1g of a mixture;
(2) Performing melt heat treatment on the mixture at 1700 ℃ for 1h in nitrogen atmosphere, pouring glass in a mold, annealing and cooling, keeping the temperature at 550 ℃ for 60min, and cooling to room temperature to obtain the metal ion (Ag) containing material + ) The high borosilicate glass of (1).
(3) Finally, the obtained metal ion (Ag) is added + ) The high borosilicate glass was irradiated with X-rays (CuK α, λ = 0.1541691m, 50kv, 50ma) at room temperature for 30min, then heat-treated at 400 ℃ for 60min under nitrogen atmosphere, and then cooled to room temperature, to obtain 61.8g of high borosilicate glass containing metal nanoparticles. The generated metal nanoparticles are characterized by ultraviolet-visible absorption spectrum, as shown in fig. 1, it can be found that the spectral curve shows the characteristic peak of the metal nanoparticles, the wavelength is stable, and the absorption band is about 400nm, under the condition, the metal nanoparticles with good stability can be prepared in the high borosilicate glass.
Example 2:
a method for synthesizing metal nanoparticles in high borosilicate glass, characterized by: the preparation method comprises the following steps:
(1) 98.35g of high borosilicate glass batch and 0.2361g of AgNO 3 Then adding 1.1g of SnO reducing agent, mixing in equal proportion, and grinding and mixing in a ceramic mortar for 30min to obtain 98.6g of a mixture;
(2) Performing melt heat treatment on the mixture at 1700 ℃ for 1h in nitrogen atmosphere, pouring glass in a mold, annealing and cooling, keeping the temperature at 550 ℃ for 60min, and cooling to room temperature to obtain the metal ion (Ag) containing material + ) The high borosilicate glass of (1).
(3) Finally, the obtained metal ion (Ag) is added + ) The high borosilicate glass was irradiated with X-rays (CuK α, λ = 0.1541691m, 50kv, 50ma) at room temperature for 30min, then heat-treated at 600 ℃ for 60min under nitrogen atmosphere, and then cooled to room temperature, to obtain 57.2g of high borosilicate glass containing metal nanoparticles. The generated metal nanoparticles are characterized by ultraviolet-visible absorption spectrum, as shown in fig. 2, it can be found that the spectral curve shows the characteristic peak of the metal nanoparticles, the wavelength is stable, and the absorption band is about 404nm, under the condition, the metal nanoparticles with good stability can be prepared in the high borosilicate glass.
Example 3:
a method for synthesizing metal nanoparticles in high borosilicate glass, comprising: the preparation method comprises the following steps:
(1) 98.42g of a high borosilicate glass batch with 0.1259g of AgNO 3 Then adding 1.7g of SnO reducing agent, mixing in equal proportion, and grinding and mixing in a ceramic mortar for 30min to obtain 98.5g of a mixture;
(2) Performing fusion heat treatment on the mixture at 1700 ℃ for 1h in nitrogen atmosphere, pouring glass in a mold, annealing and cooling, keeping the temperature at 550 ℃ for 60min, and cooling to room temperature to obtain the metal ion (Ag) containing material + ) The high borosilicate glass of (1).
(3) Finally, the obtained metal ion (Ag) is added + ) The high borosilicate glass is irradiated by X-ray (CuKa, lambda =0.15416nm,50kV and 50mA) for 30min at room temperature, then is subjected to high-temperature heat treatment at 600 ℃ for 60min under the atmosphere of nitrogen, and is cooled to room temperature, so that 55.7g of the high borosilicate glass containing metal nano particles is obtained. The generated metal nanoparticles are characterized by ultraviolet-visible absorption spectrum, as shown in fig. 3, it can be found that the spectral curve shows the characteristic peak of the metal nanoparticles, the wavelength is stable, and the absorption band is about 400nm, under the condition, the metal nanoparticles with good stability can be prepared in the high borosilicate glass.
Example 4:
a method for synthesizing metal nanoparticles in high borosilicate glass, characterized by: the preparation method comprises the following steps:
(1) 98.8g of a high borosilicate glass batch was mixed with 0.5589g of Cu 2 O, then 0.6g of CeO is added 2 A reducing agent, which is ground and mixed in a ceramic mortar for 30min to obtain 97.9g of a mixture;
(2) Performing melt heat treatment on the mixture at 1750 ℃ for 1.5h in an argon atmosphere, pouring glass in a mold, annealing and cooling, keeping the temperature at 550 ℃ for 70min, and cooling to room temperature to obtain a metal ion (Cu) containing material + ) The high borosilicate glass of (1).
(3) Finally, the obtained metal ion (Cu) is added + ) The high borosilicate glass is irradiated by X-ray (CuKa, lambda = 0.1541691m, 50kV, 50mA) for 40min at room temperature, then is subjected to high-temperature heat treatment at 700 ℃ for 50min under argon atmosphere, and is cooled to room temperature, thus obtaining 62.4g of high borosilicate glass containing metal nano particles. The generated metal nano-particles are characterized by ultraviolet-visible absorption spectrum, and the spectral curve shows the characteristic peak of the metal nano-particles, the peak shape is stable, and the metal nano-particles with good stability can be prepared in the high borosilicate glass under the condition.
Comparative example 1:
the comparative example adopts common soda-lime-silica glass, and the raw materials introduced into each group select reagent-grade SiO 2 ，Na 2 CO 3 ，CaCO 3 And Al (OH) 3 Weigh 732gSiO 2 、261gNa 2 CO 3 、181gCaCO 3 And 19gAl (OH) 3 And mixing to obtain the soda-lime-silica glass batch. The sodium-calcium-silicon glass has the theoretical mass composition (wt%) of SiO 2 :73.2，Na 2 O:15.3，CaO:10.2，Al 2 O 3 :1.3。
99.92g of ordinary soda-lime-silica glass batch and 0.1259g of AgNO 3 Grinding and mixing in a ceramic mortar for 30min to obtain 97.3g of a mixture; performing melting heat treatment at 1400 deg.C for 3h, pouring into glass in a mold, annealing, cooling, keeping at 550 deg.C for 70min, and cooling to room temperature to obtain metal ion (Ag) + ) The soda-lime-silica glass of (1).
Containing Ag + After the common soda-lime-silica glass is irradiated by X-rays (CuK alpha, lambda =0.15416nm,50kV and 50mA) for 30min, ag atoms are generated, the glass is heated to 420 ℃ and is kept for 60min to obtain 68.7g of soda-lime-silica glass containing Ag nano particles, and the glass has an obvious absorption peak at about 405 nm. As shown in FIG. 4, in the ordinary soda-lime-silica glass, ag nano-particles are generated at 420 ℃, the glass has a characteristic yellow color, but when the glass is heated at about 560 ℃, the Ag nano-particles disappear, and an obvious absorption peak at about 405nm is resolved.
The physicochemical properties and characteristic absorption peaks of the Ag nanoparticles of the high borosilicate glass containing Ag nanoparticles are more stable as can be seen by comparing example 2 with comparative example 1.
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 preparing high borosilicate glass containing metal nano-particles is characterized by comprising the following steps:
(1) Mixing the following components in parts by mass: 940-997 parts of high borosilicate glass batch, 0.2-10 parts of metal compound micro powder with the particle size of 200-1600 meshes and 2-50 parts of reducing agent to obtain a premix; the metal compound of the metal compound micro powder is AgNO 3 、HAuCl 4 ·4H 2 O、Cu 2 One or more of O; the above-mentionedThe reducing agent is SnO or Sb 2 O 5 、CeO 2 One or more of; the high borosilicate glass batch is composed of the following components in parts by mass: 780-850 parts of silicon dioxide, 170-270 parts of boric acid, 68-172 parts of sodium carbonate, 0-76 parts of aluminum hydroxide and 0-90 parts of calcium carbonate;
(2) Melting and heat-treating the premix obtained in the step (1) at 1450-1800 ℃ for 1-4 h under a protective atmosphere A, injecting the obtained glass melt into a mold, annealing at 400-550 ℃, keeping the temperature for 30-90 min, and cooling to room temperature to obtain glass containing metal ions;
(3) And (3) irradiating the glass containing the metal ions in the step (2) by X-ray at room temperature for 30-120 min, then carrying out heat treatment at 400-700 ℃ for 30-90 min under the protective atmosphere B, and cooling to obtain the high borosilicate glass containing the metal nanoparticles.
2. The method of preparing a high borosilicate glass containing metal nanoparticles according to claim 1, wherein: the metal compound of the metal compound micro powder in the step (1) is AgNO 3 、Cu 2 One or two of O.
3. The method for preparing high borosilicate glass containing metal nanoparticles according to claim 1, wherein the components are mixed in the following parts by mass in step (1): 975-994 parts of high borosilicate glass batch, 0.8-5 parts of metal compound micro powder with the grain diameter of 200-1600 meshes and 5-20 parts of reducing agent.
4. The method of preparing a high borosilicate glass containing metal nanoparticles according to claim 1, wherein: in the step (1), the reducing agent is SnO or CeO 2 One or two of them.
5. The method of preparing a high borosilicate glass containing metal nanoparticles according to claim 1, wherein the method comprises: the high borosilicate glass batch in the step (1) comprises 788 parts of silicon dioxide, 226 parts of boric acid, 97 parts of sodium carbonate, 30 parts of aluminum hydroxide and 5 parts of calcium carbonate.
6. The method of preparing a high borosilicate glass containing metal nanoparticles according to claim 1, wherein: the temperature of the melting heat treatment in the step (2) is 1500-1750 ℃, and the time is 1-2 h.
7. The method of preparing a high borosilicate glass containing metal nanoparticles according to claim 1, wherein: the protective atmosphere A in the step (2) or the protective atmosphere B in the step (3) is a nitrogen or argon atmosphere.
8. The method of preparing a high borosilicate glass containing metal nanoparticles according to claim 1, wherein: the parameters of the X-ray irradiation in step (3) are CuK α, λ =0.15416nm,50kv,50ma.
9. The method of preparing a high borosilicate glass containing metal nanoparticles according to claim 1, wherein the method comprises: the X-ray irradiation time of the glass powder containing metal ions in the step (3) is 30-60 min.
10. The method of preparing a high borosilicate glass containing metal nanoparticles according to claim 1, wherein: the heat treatment condition in the step (3) is heat treatment at 500-600 ℃ for 30-60 min.
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