CN110590171B - High-strength high-temperature-resistant glass for laboratory and preparation method thereof - Google Patents
High-strength high-temperature-resistant glass for laboratory and preparation method thereof Download PDFInfo
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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
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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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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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
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
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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
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
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Abstract
The invention discloses high-strength high-temperature-resistant glass for a laboratory and a preparation method thereof, and belongs to the field of inorganic materials. The glass developed by the invention adopts lithium disilicate as a glass matrix, and silicon microcrystal particles, inert silicon compounds, fluxing agents and nucleating agents, the surfaces of which are coated with nano rare earth oxides, are added; when the product is prepared, the raw materials are firstly prepared, then the liquid phase precipitation is adopted to coat the nano rare earth oxide on the surface of the silicon microcrystal, and finally the high-strength high-temperature-resistant glass for the laboratory is prepared by high-temperature firing. The product obtained by the invention has good mechanical property and high temperature resistance.
Description
Technical Field
The invention relates to the field of inorganic materials, in particular to high-strength high-temperature-resistant glass for laboratories and a preparation method thereof.
Background
In a common laboratory, glass is used as a table top and the like, and has absolute advantages in the aspects of attractiveness, practicability, convenience in maintenance and management and the like; because laboratory experiment conditions are complicated, in the experimental process, foreign matters often directly impact glass, various heated utensils are also in direct contact with cooled glass, the requirements of safety and protection are met, and higher requirements are provided for the strength and high temperature resistance of glass used in a laboratory, particularly table glass.
The physical tempering is to heat the glass to a softening temperature and then rapidly cool the glass, and the surface of the glass is firstly contracted and solidified by contacting cold air. The volume of the surface layer of the glass after cooling is larger than that of the surface layer before heating, heat conduction is carried out through the surface of the glass inside the glass, the cooling rate is slow, the bond length can be restored to the original state, and the volume of the inside of the glass is the same as that of the original glass, so that the surface of the glass has certain compressive stress. Because the 'volume difference' generated stress is obtained by depending on the principle of expansion with heat and contraction with cold, the physically toughened glass has lower surface compressive stress, shallower depth of the compressive stress and small strength of the glass with unit thickness, and can meet the requirement of the strength of the table top only by a certain thickness; and the low internal tensile stress of glass grid structure's tolerance is low, and when tensile stress was too big, when receiving the striking, the branching broke easily takes place, and the piece is little and splash far, and the potential safety hazard is big.
Disclosure of Invention
The invention aims to provide high-strength high-temperature-resistant glass for a laboratory and a preparation method thereof, and aims to overcome the defects of insufficient strength and high-temperature resistance of a glass table top in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
high-strength high-temperature-resistant glass for laboratories, wherein silicon microcrystals are dispersed in the glass; the addition amount of the silicon microcrystal is not more than 20 percent of the mass of the glass matrix.
According to the technical scheme, the silicon microcrystal particles are added into a glass system, and the silicon microcrystal particles are used as a microcrystal particle reinforcing phase in a glass phase, so that the silicon microcrystal particle reinforcing phase contributes to the improvement of the integral impact resistance of glass; on the other hand, can form the grain boundary between silicon microcrystal particle and the glass substrate, can have tiny clearance between crystal and the crystal promptly, and the existence of this grain boundary can play good buffering effect, not only can cushion the high temperature to the inside thermal shock of glass crystal, can cushion the impact of stress in the twinkling of an eye simultaneously, makes the intensity and the high temperature resistance performance of product obtain promoting simultaneously.
Further, the average particle size of the silicon microcrystal particles dispersed in the glass is 0.01-50 μm; the average specific surface area is 0.5 to 20m2/g。
According to the technical scheme, the silicon microcrystal particles with special particle sizes and specific surface areas are adopted, the surface activity of the silicon microcrystal particles with the size grades is high, and the interaction force between the silicon microcrystal particles and a glass phase is stronger when the silicon microcrystal particles are dispersed in the glass phase, so that the bonding property of a melting system is favorably improved, the internal stress of a product is increased, and the mechanical property is improved.
Further, the average grain size of the silicon microcrystal grains is 1-500 nm; the surface of the silicon microcrystal particles is coated with nano rare earth oxide.
According to the technical scheme, the nano rare earth oxide is further coated on the surface of the silicon microcrystal particle, because when the silicon microcrystal particle is fused and sintered with a glass matrix at a high temperature, part of the surface of the silicon microcrystal or part of the surface of the silicon microcrystal is easy to form a whole with the glass matrix, so that a crystal boundary between the silicon microcrystal and the glass matrix disappears, and the addition of the nano rare earth oxide can achieve a good blocking effect; furthermore, the addition of rare earth oxides allows the "intrusion" of microcrystalline silicon particles into the glass matrix.
Further, the average thickness of the nano rare earth oxide coated on the surface of the silicon microcrystal particle is 1-50 nm; the rare earth oxide is any one of lanthanum oxide, cerium oxide, yttrium oxide and praseodymium oxide.
Further, the glass comprises an inert silicon compound accounting for 1-10% of the total mass of the glass substrate; the inert silicon compound is silicon carbide and/or silicon nitride.
According to the technical scheme, the inert silicon compound with good compatibility with the matrix is further introduced into the glass matrix, and the inert silicon compound can be invaded into the glass matrix to form a volume difference with silicon microcrystal particles invaded into the glass matrix, so that an extrusion effect is generated, compression stress is formed inside the glass, the tissues or cracks are delayed to diffuse into the glass, and the strength of the glass is finally improved.
Further, the glass substrate is lithium disilicate glass.
Furthermore, the glass comprises 1-5% of spherical zinc borate and 1-3% of hydroxyapatite, wherein the mass of the spherical zinc borate is the mass of the glass matrix.
According to the technical scheme, spherical zinc borate and hydroxyapatite are added into a glass substrate, on one hand, when the zinc borate and the hydroxyapatite are mixed and treated at high temperature, the zinc borate can accelerate the decomposition of the hydroxyapatite, so that the decomposition temperature of the hydroxyapatite is close to the crystal form transition temperature of the zinc borate, the zinc borate can accelerate the decomposition of the hydroxyapatite, the zinc borate and the hydroxyapatite are subjected to heat absorption in the crystal form transition process, the zinc borate and the hydroxyapatite absorb heat in the decomposition process, the zinc borate and the hydroxyapatite counteract each other, large heat absorption and heat release peaks of the glass substrate in the high-temperature sintering process are avoided, the glass sintering process is facilitated, the mixing of different crystal phases in the glass is realized, the internal defects caused by the shrinkage and expansion caused by the intense heat release and heat absorption reactions in the high-temperature melting process are avoided, and the high-temperature resistance and the mechanical property of the product are effectively improved; in addition, after the hydroxyapatite is decomposed, the hydroxyapatite can be further refined, a crystal boundary is formed between the hydroxyapatite and a glass matrix, a good buffering effect is achieved, and compared with common zinc borate, the appearance of the spherical zinc borate is spherical or ellipsoidal, the spherical zinc borate is more uniformly mixed with all components in the material mixing process, a more compact structure can be obtained in the sintering process, and the high-temperature resistance of the product is further improved.
A preparation method of high-strength high-temperature-resistant glass for laboratories comprises the following specific preparation steps:
(1) preparing raw materials;
(2) preparing silicon microcrystal particles coated with rare earth oxide on the surface;
(3) and (5) firing the product.
Further, the preparation method of the high-strength high-temperature-resistant glass for the laboratory comprises the following specific preparation steps:
(1) preparing raw materials;
(2) preparing the silicon microcrystal particles coated with the rare earth oxide on the surface:
A. coating dopamine on the surface of the silicon microcrystal;
B. dispersing the silicon microcrystal coated with dopamine in a rare earth salt solution, and adjusting the pH value to precipitate the rare earth salt;
C. roasting the precipitate at low temperature of 300 ℃ to obtain silicon microcrystal particles with surfaces coated with rare earth oxides;
(3) and (5) firing the product.
Further, a preparation method of the high-strength high-temperature-resistant glass for the laboratory comprises the following specific preparation steps:
(1) preparing raw materials;
(2) preparation of silicon microcrystal particles coated with rare earth oxide:
A. coating dopamine on the surface of the silicon microcrystal;
B. dispersing the silicon microcrystal coated with dopamine in a rare earth salt solution, and adjusting the pH value to precipitate the rare earth salt;
C. roasting the precipitate at low temperature of 300 ℃ to obtain silicon microcrystal particles with surfaces coated with rare earth oxides;
(3) firing a product:
A. uniformly mixing the silicon microcrystal particles coated with the rare earth oxide on the surface, lithium disilicate glass, an inert silicon compound, a fluxing agent, a nucleating agent, spherical zinc borate and hydroxyapatite, melting at a high temperature, firing, and cooling to obtain the high-strength high-temperature-resistant glass for the laboratory.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Selecting the average grain diameter of 0.01 mu m; the average specific surface area was 0.5m2Silicon microcrystal particles and a dopamine solution with the mass concentration of 2g/L are mixed according to the mass ratio of 1: 10, adjusting the pH value to 7.2, stirring and mixing for 10min at the rotating speed of 300r/min by using a stirrer, filtering, washing and drying to obtain the dopamine-coated silicon microcrystal particles;
coating silicon microcrystal particles coated with dopamine and a rare earth salt solution with the mass fraction of 2% in a mass ratio of 1: 5, mixing, dropwise adding ammonia water to adjust the pH value to 7.5 under the stirring state at the rotating speed of 300r/min, and filtering, washing and drying to obtain the silicon microcrystal with the surface coated with the rare earth precursor;
then transferring the silicon microcrystal of which the surface is coated with the rare earth precursor into a muffle furnace, roasting at the low temperature of 300 ℃ for 1h under the protection of nitrogen, cooling to room temperature along with the furnace, and discharging to obtain silicon microcrystal particles of which the surface is coated with rare earth oxide; the average thickness of the nano rare earth oxide coated on the surface of the silicon microcrystal particle is 1 nm; the rare earth oxide is lanthanum oxide;
according to the weight parts, 100 parts of lithium disilicate glass, 1 part of silicon microcrystal particles coated with rare earth oxides on the surfaces, 0.1 part of inert silicon compound, 0.1 part of cosolvent, 0.1 part of nucleating agent, 1 part of spherical zinc borate and 1 part of hydroxyapatite are taken in sequence, uniformly mixed, melted at a high temperature, fired, cooled and formed, and then the high-strength high-temperature resistant glass for laboratories is obtained; the inert silicon compound is silicon carbide.
Example 2
Selecting the average grain diameter of 20 mu m; the average specific surface area is 10m2Silicon microcrystal particles and a dopamine solution with the mass concentration of 3g/L are mixed according to the mass ratio of 1: 50, adjusting the pH value to 7.2, stirring and mixing for 50min at the rotating speed of 400r/min by using a stirrer, filtering, washing and drying to obtain the dopamine-coated silicon microcrystal particles;
coating silicon microcrystal particles coated with dopamine and a rare earth salt solution with the mass fraction of 8% in a mass ratio of 1: 15, adding ammonia water dropwise to adjust the pH value to 7.8 under the stirring state at the rotating speed of 400r/min, and filtering, washing and drying to obtain the silicon microcrystal with the surface coated with the rare earth precursor;
then transferring the silicon microcrystal of which the surface is coated with the rare earth precursor into a muffle furnace, roasting at the low temperature of 300 ℃ for 2 hours under the protection of nitrogen, cooling to room temperature along with the furnace, and discharging to obtain silicon microcrystal particles of which the surface is coated with rare earth oxide; the average thickness of the nano rare earth oxide coated on the surface of the silicon microcrystal particle is 20 nm; the rare earth oxide is cerium oxide;
according to the weight parts, 110 parts of lithium disilicate glass, 10 parts of silicon microcrystal particles coated with rare earth oxides on the surfaces, 2.0 parts of inert silicon compound, 0.2 part of cosolvent, 0.2 part of nucleating agent, 2 parts of spherical zinc borate and 2 parts of hydroxyapatite are sequentially mixed, melted at a high temperature, fired and cooled to form the high-strength high-temperature-resistant glass for the laboratory, wherein the inert silicon compound is silicon nitride.
Example 3
Selecting the average grain diameter of 50 mu m; the average specific surface area is 20m2Silicon microcrystal particles and a dopamine solution with the mass concentration of 5g/L are mixed according to the mass ratio of 1: 100, adjusting the pH value to 7.2, stirring and mixing for 60min at the rotating speed of 500r/min by a stirrer, filtering, washing and drying,obtaining silicon microcrystal particles coated with dopamine;
coating silicon microcrystal particles coated with dopamine and a rare earth salt solution with the mass fraction of 10% in a mass ratio of 1: 20, dripping ammonia water to adjust the pH value to 8.0 under the stirring state with the rotating speed of 500r/min, and then filtering, washing and drying to obtain the silicon microcrystal with the surface coated with the rare earth precursor;
then transferring the silicon microcrystal of which the surface is coated with the rare earth precursor into a muffle furnace, roasting at the low temperature of 300 ℃ for 3h under the protection of nitrogen, cooling to room temperature along with the furnace, and discharging to obtain silicon microcrystal particles of which the surface is coated with rare earth oxide; the average thickness of the nano rare earth oxide coated on the surface of the silicon microcrystal particle is 50 nm; the rare earth oxide is yttrium oxide;
according to the weight parts, 120 parts of lithium disilicate glass, 20 parts of silicon microcrystal particles coated with rare earth oxides on the surfaces, 5.0 parts of inert silicon compound, 0.3 part of cosolvent, 0.3 part of nucleating agent, 12 parts of spherical zinc borate and 6 parts of hydroxyapatite are taken in sequence, uniformly mixed, melted at a high temperature and fired, cooled and formed, and then the high-strength high-temperature resistant glass for laboratories is obtained; the inert silicon compound is silicon carbide.
Comparative example 1
This comparative example is different from example 1 in that the surface of the silicon microcrystal is not coated with the rare earth oxide, and the rest of the conditions are the same as example 1.
Comparative example 2
This comparative example differs from example 1 in that: the conditions were the same as in example 1 except that no silicon crystallite particles were added.
Comparative example 3
This comparative example differs from example 1 in that: the inert silicon compound was not added, and the remaining conditions were the same as in example 1.
Comparative example 4
This comparative example differs from example 1 in that: the spherical zinc borate was not added, and the other conditions were the same as in example 1.
The products obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to performance tests, and the specific test methods and test results were as follows:
taking a test sample with the specification of 3mm x 100mm as an experimental object, respectively placing the products of the examples and the comparative examples in a hollow frame, fixing the edges, sequentially impacting 200g of steel balls from a free falling body 30cm above a glass surface nine-square grid, gradually increasing the height by 5cm, impacting 2 times at each height point, taking the highest non-cracking point as a strength value, and measuring the impact resistance;
taking a test sample with the specification of 3mm 400mm 200mm as an experimental object, refrigerating the products of the examples and the comparative examples in a refrigerator at 4 ℃ for 3h, taking out the products, splashing hot water preheated to different temperatures onto the surface of the glass, starting from 40 ℃, returning the glass to the refrigerator for refrigerating again after each splashing is finished, and after taking out the glass again, preheating the temperature of the hot water to be 5 ℃ higher than that of the last splashing hot water until the glass cracks, wherein the cracking temperature represents the high temperature resistance of the products;
the specific test results are shown in table 1:
table 1: product performance test meter
| Impact resistance/cm | High temperature resistance/. degree.C | |
| Example 1 | 45 | 85 |
| Example 2 | 50 | 95 |
| Example 3 | 45 | 90 |
| Comparative example 1 | 35 | 70 |
| Comparative example 2 | 30 | 65 |
| Comparative example 3 | 35 | 75 |
| Comparative example 4 | 35 | 65 |
The detection results in table 1 show that, in comparative example 1, since the rare earth oxide is not coated on the surface of the silicon microcrystal, part of silicon microcrystal particles and the glass substrate are adhered into a whole, and a good crystal boundary is not formed, the mechanical property and the high temperature resistance of the product are remarkably reduced; in contrast, in comparative example 2, since the silicon microcrystal particles are not added, the performance is further deteriorated on the basis of comparative example 1; in the comparative example 3, as the inert silicon compound is not added, the silicon microcrystal particle only acts on the basis of single silicon microcrystal particle, and the silicon microcrystal particle and the inert silicon compound do not form good interaction, so that the product performance is also reduced to a certain extent; in contrast, comparative example 4 lacks the interaction with hydroxyapatite due to no addition of spherical zinc borate, thereby affecting the mechanical properties and high temperature resistance of the product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference thereto is therefore intended to be embraced therein.
Claims (5)
1. The high-strength high-temperature-resistant glass for the laboratory is characterized in that silicon microcrystals are dispersed in the glass; the addition amount of the silicon microcrystal is not more than 20% of the mass of the glass matrix;
the average particle size of the silicon microcrystal particles dispersed in the glass is 0.01-50 mu m; the average specific surface area is 0.5 to 20m2/g；
The average grain size of the silicon microcrystal grains is 1-500 nm; the surfaces of the silicon microcrystal particles are coated with nano rare earth oxide;
the average thickness of the nano rare earth oxide coated on the surface of the silicon microcrystal particle is 1-50 nm; the rare earth oxide is any one of lanthanum oxide, cerium oxide, yttrium oxide and praseodymium oxide.
2. The high-strength high-temperature-resistant glass for the laboratory according to claim 1, wherein the glass comprises an inert silicon compound in an amount of 1-10% by mass of the total mass of a glass substrate; the inert silicon compound is silicon carbide and/or silicon nitride.
3. The high-strength high-temperature-resistant glass for laboratories according to any one of claims 1 or 2, wherein the glass substrate is lithium disilicate glass.
4. The high-strength high-temperature-resistant glass for the laboratory according to claim 1, wherein the glass comprises 1-5% by mass of a glass matrix of spherical zinc borate and 1-3% by mass of a glass matrix of hydroxyapatite.
5. The preparation method of the high-strength high-temperature-resistant glass for the laboratory according to claim 1, which is characterized in that: the preparation method comprises the following specific steps:
(1) preparing raw materials;
(2) preparation of silicon microcrystal particles coated with rare earth oxide:
A. coating dopamine on the surface of the silicon microcrystal;
B. dispersing the silicon microcrystal coated with dopamine in a rare earth salt solution, and adjusting the pH value to precipitate the rare earth salt;
C. roasting the precipitate at low temperature of 300 ℃ to obtain silicon microcrystal particles with surfaces coated with rare earth oxides;
(3) firing a product:
A. uniformly mixing the silicon microcrystal particles coated with the rare earth oxide on the surface, lithium disilicate glass, an inert silicon compound, a fluxing agent and a nucleating agent, melting at a high temperature, firing, and cooling to obtain the high-strength high-temperature-resistant glass for the laboratory.
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| CN108164148A (en) * | 2017-12-30 | 2018-06-15 | 常州市奥普泰科光电有限公司 | A kind of preparation method of low-temperature sintering type devitrified glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US2561818A (en) * | 1945-01-29 | 1951-07-24 | Saint Gobain | Electrolytic method of protecting the wall of a glass furnace |
| CN1054055A (en) * | 1990-01-16 | 1991-08-28 | E.I.内穆尔杜邦公司 | Metaphosphate glass composition |
| CN101580343A (en) * | 2009-06-18 | 2009-11-18 | 中南大学 | Rare earth-mixing high strength lithium bisilicate sitall material and preparation method thereof |
| CN101812678A (en) * | 2010-03-05 | 2010-08-25 | 北京化工大学 | Method for preparing composite material coated with silver on surface through dopamine |
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