CN112174516B - Nano-particle glass composite material, preparation thereof and application thereof in glass - Google Patents
Nano-particle glass composite material, preparation thereof and application thereof in glass Download PDFInfo
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- CN112174516B CN112174516B CN202011121848.1A CN202011121848A CN112174516B CN 112174516 B CN112174516 B CN 112174516B CN 202011121848 A CN202011121848 A CN 202011121848A CN 112174516 B CN112174516 B CN 112174516B
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/026—Pelletisation or prereacting of powdered raw materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The invention belongs to the technical field of nano materials and glass preparation, and particularly discloses a nano particle glass composite material, and preparation and application thereof in glass. Uniformly mixing nano particles and glass powder in molten salt in a high-energy physical dispersion mode, dissolving salt in a uniformly mixed block by using a solvent, and filtering, drying and grinding to obtain a powdery nano particle composite parent metal; the nano-particle composite parent metal is pretreated and then added into liquid glass in a mechanical stirring mode, and novel glass can be prepared. The fused salt can remove an oxide layer on the surface of the nano-particles, reduce the interface energy, and enable the nano-particles to form a uniformly distributed and stable nano-composite material system in the glass, thereby improving the strength and fracture toughness of the glass.
Description
Technical Field
The invention relates to the technical field of nano materials and glass preparation, in particular to a nano particle glass composite material, and preparation and application thereof in glass.
Background
Glass can be broadly defined as any amorphous solid material that has significant social value for its application in everyday life and industry. However, due to their inherent brittleness, conventional glasses have very low fracture toughness, which greatly limits their use as structural materials. In recent years, the rapid development of nanotechnology makes the application of nano materials more extensive, and the nano materials are added into the traditional materials based on the characteristics of the nano materials, so that the performance of the materials can be effectively improved. At present, although it has been verified theoretically that the glass with high strength and high fracture toughness can be formed by adding the nanoparticles to the glass, it is very difficult to uniformly disperse the nanoparticles into the liquid glass matrix in the conventional processing method.
Therefore, proper processing modification of the nanoparticles is required to improve the dispersibility of the nanoparticles in the liquid glass matrix, so that the strength and fracture toughness of the prepared glass are effectively improved.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a nanoparticle glass composite material, its preparation and application in glass, which improves the dispersibility of the nanomaterial in the liquid glass matrix, and adds the nanomaterial into the liquid glass to prepare a novel glass with high strength and high fracture toughness.
To achieve the above and other related objects, a first aspect of the present invention provides a method for preparing a nanoparticle glass composite, comprising: adding the nanoparticles and the glass powder into high-temperature liquid molten salt, uniformly mixing the nanoparticles and the glass powder in a high-energy ultrasonic dispersion mode to obtain a molten salt system, solidifying the molten salt system into a block, dissolving salt in the block molten salt system by using a solvent, and filtering and drying to obtain the nanoparticle glass composite material.
Further, the high-energy super-energy dispersion mode is as follows: putting salt into a glass smelting container, heating and melting to obtain high-temperature liquid molten salt, then adding nano particles and glass powder, putting a tool head of an ultrasonic transducer into the glass smelting container, and carrying out ultrasonic stirring and dispersion.
Optionally, the salt is selected from at least one of fluoride, chloride, cyanide and hydride salts of alkali or alkaline earth metals; preferably, the alkali metal is at least one selected from Li, na and K, and the alkaline earth metal is at least one selected from Mg, ca and Ba.
Optionally, the melting point of the salt is 300 ℃ or more lower than the melting point of the glass powder. The melting point of the nanoparticles is generally higher than that of the glass powder, and therefore, the melting point of the salt is 300 ℃ and above lower than that of the glass powder, so as to ensure that the temperature of the high-temperature liquid molten salt is lower than that of the glass powder and the nanoparticles, and thus the glass powder and the nanoparticles are prevented from being melted.
Optionally, the solvent is a solvent that does not react with the nanoparticles, the glass powder, and is capable of dissolving a salt.
Optionally, the solvent is selected from at least one of water and ethanol; preferably, the solvent is deionized water.
Alternatively, theThe nanoparticles are selected from silicon carbide (SiC) and aluminum oxide (Al) 2 O 3 ) And tungsten carbide (WC).
Optionally, the glass powder is silicate mineral powder, and the main component of the glass powder is silicate double salt.
Optionally, the amplitude of the ultrasonic transducer is not less than 60 μm. The ultrasonic power exceeds the interfacial energy between the nanoparticles, thereby breaking up the nanoparticles in an agglomerated state.
Optionally, the ultrasonic stirring dispersion time is not less than 30min.
Optionally, the volume ratio of the nanoparticles, the glass powder and the high-temperature liquid molten salt is 0.01-0.5: 1: 5-8.
Further, the nanoparticle glass composite material is ground to obtain a powdery nanoparticle glass composite material.
In a second aspect, the present invention provides a nanoparticle glass composite material prepared by the preparation method according to the first aspect.
The third aspect of the invention provides a method for preparing glass, wherein the nanoparticle glass composite material of the second aspect is added into liquid glass, and the liquid glass is obtained by cooling and solidifying after being uniformly stirred.
Further, heating and melting glass powder under the rare gas protective atmosphere to obtain the liquid glass.
Further, the addition amount of the nano-particle glass composite material is 30-50% of the weight of the glass powder.
The fourth aspect of the invention provides a glass produced by the production method according to the third aspect.
As described above, the nanoparticle glass composite material of the present invention, the preparation thereof and the application thereof in glass have the following beneficial effects:
according to the invention, the high-temperature liquid molten salt can dissolve an oxide film on the surface of the nano particles, so that the interface energy is reduced, the uniform mixing of the nano particles and the glass powder is promoted, a uniformly distributed and stable nano particle glass composite material system is formed, after the molten salt system is solidified into a block, the nano particle glass composite material is uniformly embedded in the solid molten salt, the salt is dissolved, filtered and dried through a solvent, and then the nano particle glass composite material solid is obtained. The nano-particle glass composite material is used for preparing novel glass, and can effectively improve the strength and the fracture toughness of the glass.
Drawings
Fig. 1 is a schematic view showing the structure of an ultrasonic apparatus used in the present invention.
Fig. 2 shows a potential energy curve diagram of two identical spherical nanoparticles in liquid glass.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Description of reference numerals:
The invention provides a nano-particle glass composite material and a preparation method thereof, wherein the preparation method comprises the following steps: adding the nano particles and the glass powder into high-temperature liquid molten salt, uniformly mixing the nano particles and the glass powder in a high-energy ultrasonic dispersion mode to obtain a molten salt system, solidifying the molten salt system into a block, dissolving salt in the block molten salt system by using a solvent, and filtering, drying and grinding to obtain the powdery nano particle glass composite material.
Furthermore, the volume ratio of the nano particles to the glass powder to the high-temperature liquid molten salt is 0.01-0.5: 1: 5-8.
Further, the high-energy super-energy dispersion mode is as follows: putting salt into a glass smelting container, heating and melting to obtain high-temperature liquid molten salt, then adding nano particles and glass powder, putting a tool head of an ultrasonic transducer into the glass smelting container, and carrying out ultrasonic stirring and dispersion. Wherein the amplitude of the ultrasonic transducer is not less than 60 μm, and the ultrasonic stirring dispersion time is not less than 30min. The ultrasonic power exceeds the interfacial energy between the nanoparticles, thereby breaking up the nanoparticles in an agglomerated state.
The ultrasonic device for stirring in the invention is shown in figure 1, and comprises an ultrasonic transducer 1, an amplitude transformer 2, a tool head 3, an induction coil 4 and a crucible 5, wherein the tool head 3 is cylindrical, the characteristic length (height) of the tool head in the vertical direction is not more than half of the height of the crucible 5 (glass melting container), and the characteristic length (diameter) of the tool head in the horizontal direction is 1/3-1/5 of the diameter of the crucible 5 (glass melting container).
Further, the salt is selected from at least one of fluoride salt, chloride salt, cyanide salt and hydride salt of alkali metal or alkaline earth metal; preferably, the alkali metal is at least one selected from Li, na and K, and the alkaline earth metal is at least one selected from Mg, ca and Ba.
Further, the melting point of the salt is 300 ℃ or more lower than the melting point of the glass powder. The melting point of the nanoparticles is generally higher than that of the glass powder, and therefore, the melting point of the salt is 300 ℃ and above lower than that of the glass powder, so as to ensure that the temperature of the high-temperature liquid molten salt is lower than that of the glass powder and the nanoparticles, and thus the glass powder and the nanoparticles are prevented from being melted.
The action mechanism of the nano particles uniformly dispersed in the liquid glass is as follows:
aiming at specific liquid glass, a nano particle with enough high interfacial energy and enough low van der Waals action potential in the liquid glass is selected, so that the nano particle can be uniformly distributed in the liquid glass and the agglomeration phenomenon is avoided. The mechanism by which nanoparticles satisfying this condition can be uniformly distributed in the liquid glass is as follows: the potential energy curves of two identical nanoparticles in liquid glass include three components, interfacial energy, van der waals interaction potential, and brownian energy, as shown in fig. 1.
1. Interfacial energy
At high temperatures, two nanoparticles can sinter together driven by interfacial energy when they come into contact. In nanoparticle-liquid glassIn glass systems, when two nanoparticles approach each other until the last atomic layer of the matrix is extruded, the nanoparticle-liquid glass interface is replaced by the surface of the nanoparticles, increasing the interfacial energy W barrier ＝S(σ np -σ np-1 )＝Sσ 1 cos θ, where S is the effective area, σ np Is the surface energy of the nanoparticles, σ np-1 Is the interfacial energy between the nanoparticles and the liquid glass, σ 1 Is the surface tension of the liquid glass and θ is the contact angle of the liquid glass melt on the nanoparticle surface. The equation clearly shows that the better the wetting between the nanoparticles and the liquid glass (the smaller θ), the higher the energy barrier preventing the nanoparticles from contacting each other.
2. Van der waals' action potential
The van der waals interaction potential between two identical nanoparticles in a liquid matrix has a range of action of a certain length. The van der waals interaction potential causes an attractive force between two identical nanoparticles. Radius R 1 And R 2 The van der waals interaction potential and the interaction force of two identical nanoparticles can be expressed as:
where A is the Hamaker constant for the interaction between two identical nanoparticles in a liquid matrix. Based on Lifshitz's theory, the system Hamaker constant between media 1 and 2 between media 3 can be estimated by:
wherein epsilon 1 ，ε 2 ，ε 3 Is the static dielectric constant of the three media,. Epsilon. (iv) is the imaginary component of the media, and v is n And =2 π kT/hn. System Hamaker constant a 132 Defined as the interaction of materials 1 and 2 through medium 3, can be approximated by the formula:
wherein A is 11 ，A 22 ，A 33 Respectively, are the Hamaker constants for materials 1,2,3, respectively, to interact with themselves in vacuum, and thus the van der waals interaction potential in a nanoparticle-liquid glass system can be written as:
from equations (1-4) we can see that the van der waals interaction potential between two identical nanoparticles is always negative and that the van der waals forces between two identical nanoparticles in liquid glass are always attractive.
3. Brown energy
Since the nanoparticles are very small and move randomly under thermal fluctuations, there is brownian energy kT.
In summary, in conjunction with fig. 2, we should select a nanoparticle with a high enough interfacial energy and a low enough van der waals interaction potential in the liquid glass so that the nanoparticles can be uniformly distributed in the liquid glass without agglomeration.
Thus, the nanoparticles in the present invention are selected from silicon carbide (SiC), aluminium oxide (Al) 2 O 3 ) And tungsten carbide (WC).
Furthermore, the glass powder is silicate mineral powder, and the main component of the glass powder is silicate double salt.
Further, the solvent is a solvent that does not react with the nanoparticles and the glass powder and can dissolve a salt. Preferably, the solvent is selected from at least one of water and ethanol; more preferably, the solvent is deionized water.
According to the invention, the oxide film on the surface of the nano-particles can be dissolved through the high-temperature liquid molten salt, the interface energy is reduced, so that uniform mixing of the nano-particles and the glass powder is promoted, a uniformly distributed and stable nano-particle glass composite material system is formed, after the molten salt system is solidified into a block, the nano-particle glass composite material is uniformly embedded in the solid molten salt, the salt is dissolved, filtered and dried through the solvent, and then the nano-particle glass composite material solid is obtained.
The nano-particle glass composite material is used for preparing novel glass, and can effectively improve the strength and the fracture toughness of the glass. The preparation method of the glass comprises the following steps: heating and melting glass powder under the rare gas protective atmosphere to obtain the liquid glass, adding the nanoparticle glass composite material into the liquid glass, uniformly stirring, and cooling and solidifying to obtain the novel glass.
Further, the addition amount of the nano-particle glass composite material is 30-50% of the weight of the glass powder.
Example 1
The preparation method of the nanoparticle glass composite material in the embodiment comprises the following steps:
(1) Heating NaCl to 900 deg.c to obtain molten NaCl, and adding cordierite Al 2 O 3 -MgO-SiO 2 Adding the powder and 50nm SiC spherical nanoparticles into molten NaCl, and mixing the nanoparticles and cordierite Al 2 O 3 -MgO-SiO 2 The volume ratio of the powder to the high-temperature liquid molten salt is 0.25: 1:5, and the high-temperature high-energy ultrasonic stirring is carried out in the molten salt, the amplitude of an ultrasonic transducer is 60 mu m, and the ultrasonic time is 30min.
(2) And cooling and solidifying the molten salt system into blocks, dissolving NaCl in deionized water, filtering through filter paper, drying the rest deionized water in a drying oven at 110 ℃, and finally grinding to obtain the powdery nano-particle glass composite material.
The prepared nano-particle glass composite material is applied to glass manufacturing, and specifically comprises the following steps:
adding cordierite Al 2 O 3 -MgO-SiO 2 Adding the powder into a phi 100X180 crucible, heating to 1650 ℃ in Ar protective atmosphere, keeping the temperature for 10min to obtain liquid glass, adding the pretreated nano-particle glass composite material, wherein the adding amount of the nano-particle glass composite material is 30% of the weight of the glass powder, mechanically stirring for 30min,after cooling and solidification, the nano composite glass material system with uniformly dispersed and stable nano particles can be obtained.
Example 2
The preparation method of the nanoparticle glass composite material in the embodiment comprises the following steps:
(1) Heating NaCl to 900 deg.C to obtain molten NaCl, and mixing cordierite Al 2 O 3 -MgO-SiO 2 Adding the powder and 50nm SiC spherical nanoparticles into molten NaCl, and mixing the nanoparticles and cordierite Al 2 O 3 -MgO-SiO 2 The volume ratio of the powder to the high-temperature liquid molten salt is 0.01: 1:5, and the high-temperature high-energy ultrasonic stirring is carried out in the molten salt, the amplitude of an ultrasonic transducer is 60 mu m, and the ultrasonic time is 30min.
(2) And cooling and solidifying the molten salt system into blocks, dissolving NaCl in deionized water, filtering through filter paper, drying the rest deionized water in a drying oven at 110 ℃, and finally grinding to obtain the powdery nano-particle glass composite material.
The prepared nano-particle glass composite material is applied to glass manufacturing, and specifically comprises the following steps:
adding cordierite Al 2 O 3 -MgO-SiO 2 Adding the powder into a phi 100X180 crucible, heating to 1650 ℃ in Ar protective atmosphere, preserving the temperature for 10min to obtain liquid glass, adding the pretreated nano-particle glass composite material, wherein the adding amount of the nano-particle glass composite material is 30% of the weight of the glass powder, mechanically stirring for 30min, and cooling and solidifying to obtain a nano-composite glass material system with uniformly dispersed and stable nano-particles.
Example 3
The preparation method of the nanoparticle glass composite material in the embodiment comprises the following steps:
(1) Heating NaCl to 900 deg.c to obtain molten NaCl, and adding cordierite Al 2 O 3 -MgO-SiO 2 Adding the powder and 50nm SiC spherical nanoparticles into molten NaCl, and adding the nanoparticles and cordierite Al 2 O 3 -MgO-SiO 2 The volume ratio of the powder to the high-temperature liquid molten salt is 0.5:1: 8, and high-temperature high-energy ultrasonic stirring is carried out in the molten saltThe amplitude of the ultrasonic transducer is 65 μm, and the ultrasonic time is 40min.
(2) And cooling and solidifying the molten salt system into blocks, dissolving NaCl in deionized water, filtering through filter paper, drying the rest deionized water in a drying oven at 110 ℃, and finally grinding to obtain the powdery nano-particle glass composite material.
The prepared nano-particle glass composite material is applied to glass manufacturing, and specifically comprises the following steps:
adding cordierite Al 2 O 3 -MgO-SiO 2 Adding the powder into a phi 100X180 crucible, heating to 1650 ℃ in Ar protective atmosphere, preserving the temperature for 10min to obtain liquid glass, adding the pretreated nano-particle glass composite material, wherein the addition amount of the nano-particle glass composite material is 50% of the weight of the glass powder, mechanically stirring for 30min, and cooling and solidifying to obtain a nano-composite glass material system with uniformly dispersed and stable nano-particles.
Example 4
The preparation method of the nanoparticle glass composite material in the embodiment comprises the following steps:
(1) Heating NaCl to 900 deg.C to obtain molten NaCl, and mixing cordierite Al 2 O 3 -MgO-SiO 2 Adding the powder and 50nm tungsten carbide WC spherical nanoparticles into molten NaCl, and adding the nanoparticles and cordierite Al 2 O 3 -MgO-SiO 2 The volume ratio of the powder to the high-temperature liquid molten salt is 0.25: 1:5, and the high-temperature high-energy ultrasonic stirring is carried out in the molten salt, the amplitude of an ultrasonic transducer is 60 mu m, and the ultrasonic time is 30min.
(2) And cooling and solidifying the molten salt system into blocks, dissolving NaCl in deionized water, filtering through filter paper, drying the rest deionized water in a drying oven at 110 ℃, and finally grinding to obtain the powdery nano-particle glass composite material.
The prepared nano-particle glass composite material is applied to glass manufacturing, and specifically comprises the following steps:
adding cordierite Al 2 O 3 -MgO-SiO 2 Adding the powder into a phi 100X180 crucible, heating to 1650 ℃ in Ar protective atmosphere, and keeping the temperature for 10min to obtain the liquid glassAnd adding the pretreated nano-particle glass composite material into the glass, wherein the addition amount of the nano-particle glass composite material is 40 percent of the weight of the glass powder, mechanically stirring the mixture for 30min, and cooling and solidifying the mixture to obtain a nano-particle glass composite material system with uniformly dispersed and stable nano-particles.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (7)
1. A method of making a nanoparticle glass composite, comprising: adding nanoparticles and glass powder into high-temperature liquid molten salt, and uniformly mixing the nanoparticles and the glass powder in a high-energy ultrasonic dispersion mode to obtain a molten salt system, wherein the high-energy ultrasonic dispersion mode is as follows: putting salt into a glass smelting container, heating and melting to obtain high-temperature liquid molten salt, then adding nano particles and glass powder, putting a tool head of an ultrasonic transducer into the glass smelting container, and carrying out ultrasonic stirring and dispersion; then solidifying the molten salt system into a block, dissolving salt in the block molten salt system by using a solvent, filtering, drying and grinding to obtain a powdery nano-particle glass composite material;
the salt is selected from at least one of fluoride salt, chloride salt, cyanide salt and hydride salt of alkali metal or alkaline earth metal, the alkali metal is selected from at least one of Li, na and K, the alkaline earth metal is selected from at least one of Mg, ca and Ba, and the melting point of the salt is 300 ℃ or more lower than the melting point of the glass powder; the nano particles are selected from at least one of silicon carbide, aluminum oxide and tungsten carbide, the glass powder is silicate mineral powder, and the solvent is a solvent which does not react with the nano particles and the glass powder and can dissolve salt;
the volume ratio of the nano particles to the glass powder to the high-temperature liquid molten salt is 0.01-0.5.
2. The method of making a nanoparticle glass composite as recited in claim 1, wherein: the solvent is at least one of water and ethanol.
3. The method of making a nanoparticle glass composite as recited in claim 1, wherein: the amplitude of the ultrasonic transducer is not lower than 60 mu m;
and/or the ultrasonic stirring dispersion time is not less than 30min.
4. The nanoparticle glass composite produced by the production method according to any one of claims 1 to 3.
5. A preparation method of glass is characterized in that: adding the nanoparticle glass composite material of claim 4 into liquid glass, stirring uniformly, cooling and solidifying to obtain the glass.
6. The method for producing glass according to claim 5, characterized in that: heating and melting glass powder under the rare gas protective atmosphere to obtain the liquid glass;
and/or the addition amount of the nano-particle glass composite material is 30-50% of the weight of the glass powder.
7. Glass produced by the production method according to any one of claims 5 to 6.
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