CN111847901A - Strengthened glass articles and methods of making the same - Google Patents

Strengthened glass articles and methods of making the same Download PDF

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Publication number
CN111847901A
CN111847901A CN202010752454.XA CN202010752454A CN111847901A CN 111847901 A CN111847901 A CN 111847901A CN 202010752454 A CN202010752454 A CN 202010752454A CN 111847901 A CN111847901 A CN 111847901A
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acid
strengthened glass
glass product
glass
agent
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CN111847901B (en
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陈建章
王世军
陈磊
丁雄风
彭晓林
杨汛
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Wanjin Industrial Chibi Co Ltd
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Wanjin Industrial Chibi Co Ltd
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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
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
    • C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B11/00—Cleaning flexible or delicate articles by methods or apparatus specially adapted thereto
    • B08B11/04—Cleaning flexible or delicate articles by methods or apparatus specially adapted thereto specially adapted for plate glass, e.g. prior to manufacture of windshields
    • 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
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • 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
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The invention relates to a strengthened glass product and a preparation method thereof; the preparation method comprises the following steps: sequentially placing the glass product in a chemical toughening agent, an alkali treating agent and an acid treating agent for soaking treatment to prepare a strengthened glass product; wherein, the components of the acid treatment agent comprise fluoride salt and an acid agent which is not hydrofluoric acid; the chemical toughening agent contains potassium salt. The preparation method can safely and effectively improve the strength of the glass product, and the prepared glass product has excellent pressure resistance and impact resistance.

Description

Strengthened glass articles and methods of making the same
Technical Field
The invention relates to the field of glass processing, in particular to a strengthened glass product and a preparation method thereof.
Background
The glass product is subjected to processes such as cutting, CNC (computer numerical control) processing, loose abrasive grinding and the like in the processing process, for example, the glass product is polished, and in the process of polishing and grinding the glass product by using polishing powder, the surface of the glass is inevitably damaged to generate cracks, so that the stress concentration of the tips of microcracks is generated on the surface of the glass product, and the strength of the glass product is further reduced rapidly.
The traditional surface corrosion method can effectively remove cracks formed on the surface of the glass preparation, and reduce the phenomenon of stress concentration at the tip of a microcrack, thereby improving the strength of a glass product. At present, the traditional corrosion method uses hydrofluoric acid or hydrofluoric acid and other acids to remove cracks and improve the strength. Hydrofluoric acid is however a toxic, highly corrosive acid; in the traditional operation process of adopting hydrofluoric acid to corrode glass, a hydrofluoric acid product with high concentration needs to be further prepared into a hydrofluoric acid solution with proper concentration, and the volatility of the hydrofluoric acid is very high, so that the personnel safety of operators is not facilitated.
Therefore, how to provide a method for safely and effectively improving the strength of the glass product is of great significance.
Disclosure of Invention
Based on the above, the invention provides a strengthened glass product with high strength and a preparation method thereof, and the preparation method can safely and effectively improve the strength of the glass product.
The technical scheme of the invention is as follows.
The invention provides a preparation method of a strengthened glass product on one hand, which comprises the following steps:
providing a glass article;
placing the glass product in a chemical toughening agent for toughening treatment to obtain a toughened glass product;
placing the toughened glass product in an alkali treatment agent for alkali treatment to prepare a toughened glass intermediate;
placing the strengthened glass intermediate into an acid treatment agent for acid treatment to obtain a strengthened glass product;
wherein the chemical toughening agent contains a potassium salt; the components of the acid treatment agent include a fluoride salt and an acidic agent, which is not hydrofluoric acid.
In some embodiments, the acid treatment agent comprises the following components in percentage by mass:
1 to 20 percent of villiaumite;
5 to 10 percent of acid reagent;
0.05 to 5 percent of surfactant;
the balance being water.
In some of these embodiments, the fluorine salt is selected from at least one of sodium fluoride, potassium fluoride, and ammonium fluoride; the acidic reagent is at least one of organic acid, sulfuric acid, nitric acid, hydrochloric acid and phosphoric acid; the surfactant is a cationic surfactant.
In some of these embodiments, the conditions of the acid treatment and/or the alkali treatment are: soaking at 20-90 deg.c for 20-240 min.
In some embodiments, after the step of alkali treatment and before the step of acid treatment, the method further comprises the following steps:
and washing the strengthened glass intermediate by using acid, wherein the acid is at least one of organic acid and inorganic acid.
In some embodiments, the chemical toughening agent comprises the following components in percentage by weight:
Figure BDA0002610469500000021
in some embodiments, the temperature of the toughening treatment is 350-470 ℃, and the time of the toughening treatment is 100-500 min.
In some embodiments, the alkali treatment agent comprises the following components in percentage by mass:
10 to 30 percent of strong base;
0-10% of basic salt;
0-1% of a surfactant;
the balance being water.
In some of the embodiments, the strong base is selected from at least one of sodium hydroxide, potassium hydroxide, calcium hydroxide, and barium hydroxide; the basic salt is at least one selected from basic carbonate, basic phosphate and basic silicate.
In another aspect, the present invention provides a strengthened glass article produced by any one of the methods for producing strengthened glass described above.
Advantageous effects
In the preparation method of the strengthened glass product, firstly, a chemical toughening agent containing sylvite is used for toughening the glass product to prepare a strengthened glass product; in the toughening treatment process, ion exchange is carried out between potassium ions in potassium salt in a chemical toughening agent and sodium ions in a glass product, the sodium ions with smaller ion radius on the surface of the glass product are exchanged into potassium ions with larger ion radius through the ion exchange, and compressive stress is generated on the surface of the glass product, so that the strength of the glass is improved; then placing the toughened glass product into an alkali treatment agent for alkali treatment to prepare a toughened glass intermediate, wherein the alkali treatment agent can dissolve abrasive particles remained on the toughened glass product and can react with sodium silicate on the surface of glass at the same time so as to corrode a damage layer generated on the surface of the glass product; further placing the strengthened glass intermediate into an acid treatment agent for acid treatment, wherein the acid treatment agent comprises fluorine salt and an acid reagent which is not hydrofluoric acid, and H + of the acid reagent and F in the fluorine salt-Further forming hydrofluoric acid, wherein the hydrofluoric acid corrodes the cracks on the surface of the glass product, and the cracks formed on the surface of the glass product are effectively removed, so that the phenomenon of stress concentration at the tip of the generated microcrack is reduced, and the strength of the glass product is further improved.
In the technical scheme of the application, firstly, alkali is used for treating, and the alkali can be mixed with SiO in the glass component2The chemical reaction is generated, so that Si-O bonds in the glass are destroyed, the glass is in an active state, acid and villiaumite are adopted for acid treatment, the active state of the glass enables the effect of acid corrosion on the glass to be more thorough, the phenomenon of stress concentration at the tip of a microcrack is effectively reduced, and the purpose of strengthening the glass is achieved.
In the invention, hydrofluoric acid products are not directly used, but fluorine salt and an acidic reagent which is not hydrofluoric acid are mixed to prepare an acid treating agent and the acidic reagentH + of (2) and F in the fluorine salt-Further forming hydrofluoric acid, the acid treating agent can be prepared at present, so that operators are prevented from directly contacting high-concentration hydrofluoric acid products, the contact probability and contact time of the operators and the hydrofluoric acid are greatly reduced, the safety of the process is improved, and the personal health of the operators is guaranteed.
Further, the present invention provides a method for producing a strengthened glass, which produces a strengthened glass article having excellent pressure resistance and impact resistance.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
On one hand, the traditional glass preparation technology needs to carry out the working procedures of cutting, CNC (computer numerical control) machining, sweeping and the like, and a large amount of micro cracks are generated on the surface of a glass product in the machining process; on the other hand, in the long-term use process, the glass product is damaged by external force from the external environment or corroded by corrosive substances, and a damaged layer with microcracks is generated on the surface of the glass; the presence of these microcracks can significantly reduce the strength of the glass. Therefore, eliminating these microcracks is an effective way to increase the strength of the glass.
At present, hydrofluoric acid or mixed solution of hydrofluoric acid and other strong acids is generally adopted to corrode microcracks so as to enhance the impact resistance of glass; however, hydrofluoric acid is toxic and too oxidizing, and other strong acids, such as concentrated sulfuric acid, are generally highly corrosive, and direct use of hydrofluoric acid or strong acids can adversely affect the health of the technician.
One technical scheme is that the strength of the glass is improved by a method of machining two sides of the glass, for example, the method of flatly grinding the two sides of the glass is used for eliminating microcracks on the surface of the glass so as to enhance the strength of the glass; however, in the mechanical processing process, the glass is further damaged, scratches and the like are easy to occur, the process stability is poor, the quality of glass products is poor, the yield is reduced, and the preparation cost is increased.
Based on the method, the invention provides a method for safely and effectively improving the strength of the strengthened glass product of the glass product.
One embodiment of the present invention provides a method for producing a strengthened glass product, including the following steps S100 to 400.
S100, providing a glass product.
In step S100, the glass product may be a glass product that has not been processed and used, such as a common glass plate, an optical element glass substrate, or the like; or used glass products such as glass appliances, optical elements and the like after long-term use.
S200, placing the glass product obtained in the step S100 in a chemical toughening agent, and carrying out toughening treatment to obtain a toughened glass product; the chemical toughening agent contains potassium salt.
Further, the potassium salt is selected from at least one of nitrate, carbonate, chloride or sulfate.
In some embodiments, the chemical toughening agent in step S200 comprises the following components in percentage by weight:
Figure BDA0002610469500000051
during the toughening treatment, ion exchange is carried out between sodium ions in the glass product and potassium ions in potassium salt in the chemical toughening agent, the sodium ions with smaller ion radius on the surface of the glass product are exchanged into potassium ions with larger ion radius through the ion exchange, and the compressive stress is generated on the surface of the glass product, so that the strength of the glass product is improved.
In some embodiments, in step S200, the temperature of the toughening treatment is 350 ℃ to 470 ℃, and the time of the toughening treatment is 100min to 500 min.
And S300, placing the toughened glass product obtained in the step S200 in an alkali treatment agent for alkali treatment to obtain a strengthened glass intermediate.
In some embodiments, the alkali treatment agent in step S300 comprises the following components in percentage by mass:
10 to 30 percent of strong base;
0-10% of basic salt;
0-1% of a surfactant;
the balance being water.
The above-mentioned alkali treatment agent is capable of dissolving abrasive particles remaining on a tempered glass article and, at the same time, reacting with sodium silicate contained in the surface of the glass article to thereby corrode a damaged layer produced on the surface of the glass article.
Further, the strong base is at least one selected from the group consisting of sodium hydroxide, potassium hydroxide, calcium hydroxide and barium hydroxide; the basic salt is at least one selected from basic carbonate, basic phosphate and basic silicate.
Further, the basic salt is at least one selected from potassium carbonate, sodium dihydrogen phosphate and potassium dihydrogen phosphate.
In some of these embodiments, the surfactant is selected from an anionic surfactant or a cationic surfactant. The anionic surfactants are exemplified herein, but not limited to, the following ranges:
sulfonated fatty acid glycerides, wherein fatty acid glyceride means a sulfonated product of a mono-, di-or triester and mixtures thereof, such as caproic acid, caprylic acid, capric acid, myristic acid, lauric acid, palmitic acid, stearic acid or behenyl acid, or C9-C13Or an olefin sulfonate, or a sulfuric monoester of a monohydric alcohol, or an alkane(en) yl sulfates, for example sulfuric acid half esters selected from coconut fatty alcohol, stearyl alcohol, lauryl alcohol, myristyl alcohol, cetyl alcohol or stearyl alcohol and corresponding alkali metal salts, especially sodium salts, or salts of alkylsulfosuccinic acid, or soaps, such as saturated fatty acid soaps, for example salts of lauric acid, myristic acid, palmitic acid, stearic acid, hydrogenated erucic acid and behenic acid, and also soap mixtures, in particular from natural fatty acids, for example coconut acid, palm kernel acid or stearic acid.
The anionic surfactant of soap may be sodium salt, potassium salt, and soluble salt of organic base.
In some of these embodiments, the anionic surfactant is selected from at least one of soap, alkylbenzene sulfonate, alkyl sulfonate salt, alkyl sulfonate, alkyl sulfate, fluorine-containing fatty acid salt, polysiloxane, fatty alcohol sulfate, fatty alcohol polyoxyethylene ether sulfate, α -olefin sulfonate, fatty alcohol polyoxyethylene ether phosphate, alkylolamide, alkylsulfoacetamide, alkyl succinate sulfonate, alcohol amine alkylbenzene sulfonate, naphthenate, alkylphenol sulfonate, and polyoxyethylene monolaurate.
In some of the embodiments, in step S300, the conditions of the alkali treatment are: soaking at 20-90 deg.c for 20-240 min.
In some embodiments, after the step of alkali treatment and before the step of acid treatment, the following step S310 is further included.
S310, washing the strengthened glass intermediate by acid; the acid is at least one of an organic acid and an inorganic acid.
The alkali treatment agent remaining on the glass article is neutralized with an acid to remove the remaining alkali.
In some embodiments, in step S310, the acid solution has a concentration of 5 wt% to 50 wt%, and the acid in the acid solution is at least one selected from sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, acetic acid, oxalic acid, and citric acid.
In some of the embodiments, the acid solution in step S310 has a concentration of 10 wt%, and the acid in the acid solution is selected from hydrochloric acid.
S400, placing the strengthened glass intermediate prepared in the step S300 in an acid treatment agent for acid treatment to prepare a strengthened glass product; wherein, the components of the acid treatment agent comprise fluoride salt and an acid agent, and the acid agent is not hydrofluoric acid.
In some embodiments, the acid treatment agent in step 400 comprises the following components in mass percent:
1 to 20 percent of villiaumite;
5 to 10 percent of acid reagent;
0.05 to 5 percent of surfactant;
the balance being water.
The components of the acid treating agent comprise villiaumite and an acid agent which is not hydrofluoric acid, H + of the acid agent and F in the villiaumite-Further forming hydrofluoric acid, corroding the cracks on the damage layer by the hydrofluoric acid, and effectively removing the cracks formed on the surface of the glass, thereby reducing the phenomenon of stress concentration at the tip of the generated microcrack and effectively improving the strength of the glass product without directly using the hydrofluoric acid.
In addition, the acid treating agent can be prepared at present, so that operators are prevented from directly contacting high-concentration hydrofluoric acid products, the contact probability and contact time of the operators and hydrofluoric acid are greatly reduced, the safety of the process is improved, and the personal health of the operators is guaranteed.
Moreover, the components with specific mass percentages have obvious synergistic effect; the cationic surfactant can reduce the surface tension of the acid treatment agent on the surface of the glass, so that the contact area of the acid treatment agent and microcracks on the surface of the glass is increased, and the corrosion efficiency of hydrofluoric acid on the cracks on the damage layer is further improved.
Further, the acid treatment agent in the step 400 comprises the following components in percentage by mass:
Figure BDA0002610469500000071
in some of these embodiments, the fluorine salt is selected from at least one of sodium fluoride, potassium fluoride, and ammonium fluoride; the acidic reagent is at least one of organic acid and inorganic acid except hydrofluoric acid; the surfactant is a cationic surfactant.
The cationic surfactant is stable in an acid medium, hydrophilic radical ions of the cationic surfactant contain nitrogen atoms, and the cationic surfactant is divided into three types, namely amine salt, quaternary ammonium salt and heterocyclic type according to the position of the nitrogen atoms in molecules. The cationic surfactants are exemplified herein, but not limited to, the following ranges:
stearamidopropyl dimethylamine, stearamidopropyl diethylamine, stearamidoethyl dimethylamine, palmitamidopropyl diethylamine, palmitamidoethyl dimethylamine, behenamidopropyl diethylamine, behenamidoethyl dimethylamine, arachidamidopropyl diethylamine, arachidamidoethyl dimethylamine, diethylaminoethyl stearamide, imidazoline and its derivatives, moroxydine and its derivatives, triazine and its derivatives, etc.
Further, the acidic agent in the above-mentioned acid treatment agent is exemplified herein, but not limited to, the following ranges:
the organic acid includes carboxyl (-COOH), sulfonic acid (-SO)3H) Sulfinic acids, etc., such as: acetic acid, propionic acid, butyric acid, succinic acid, benzoic acid, oxalic acid, tartaric acid, citric acid; inorganic acids other than hydrofluoric acid such as sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, or the like.
In some of these embodiments, in step S400, the conditions of the acid treatment agent are: soaking at 20-90 deg.c for 20-240 min.
In some embodiments, step S400 further includes the following step S410 after the acid treatment.
And S410, cleaning the strengthened glass product by using a cleaning agent.
In some embodiments, the cleaning agent is an alkaline cleaning agent, such as an aqueous solution of sodium hydroxide, an aqueous solution of potassium hydroxide, or the like, and the alkaline cleaning agent is used to neutralize any acid treatment agent remaining on the glass article.
It is understood that, in step S410, the cleaning agent may also be water, and the glass product is rinsed with water until the rinsing liquid is neutral.
In the preparation method of the strengthened glass product, firstly, a chemical toughening agent containing sylvite is used for toughening the glass product to prepare the strengthened glass product; in the toughening treatment process, ion exchange is carried out between sodium ions in the glass product and potassium ions in potassium salt, the sodium ions with smaller ion radius on the surface of the glass product are exchanged into the potassium ions with larger ion radius through the ion exchange, and the compressive stress is generated on the surface of the glass, so that the strength of the glass is improved; then the toughened glass product is placed in an alkali treatment agent for treatment to prepare a toughened glass intermediate, and the alkali treatment agent can dissolve abrasive particles remained on the toughened glass product and can react with sodium silicate contained on the surface of the glass, so that a damage layer generated on the surface of the glass product is corroded; the further strengthened glass intermediate is put into an acid treatment agent for acid treatment, the components of the acid treatment agent comprise villiaumite and an acid reagent which is not hydrofluoric acid, and H + of the acid reagent and F in the villiaumite-Further forming hydrofluoric acid, wherein the hydrofluoric acid corrodes cracks on a damage layer formed on the surface of the glass product, and the microcracks on the surface prepared by the glass are effectively removed, so that the phenomenon of stress concentration at the tips of the microcracks is reduced, and the strength of the glass product is further improved.
Further, an embodiment of the present invention provides a strengthened glass product produced by the method for producing a strengthened glass according to any one of the above methods.
The glass product is sequentially subjected to toughening treatment, alkali treatment and acid treatment, sodium ions with smaller ion radius on the surface of the glass product are exchanged into potassium ions with larger ion radius through ion exchange in the toughening treatment process, and compressive stress is generated on the surface of the glass; further, the alkali treatment and the acid treatment corrode cracks on a damaged layer formed on the surface of the glass product, and the cracks formed on the surface of the glass product are effectively removed, so that the phenomenon of stress concentration at the tip of the generated microcrack is reduced, the strength of the glass product is further improved, and the glass product has excellent pressure resistance and impact resistance.
While the present invention will be described with respect to particular embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but is intended to cover by the appended claims the scope of the invention, and that certain changes in the embodiments of the invention will be suggested to those skilled in the art and are intended to be covered by the appended claims.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The strengthened glass articles and methods of making the same according to the present invention are illustrated herein, but the invention is not limited to the following examples.
Example 1
The method comprises the following specific steps.
1) Providing a glass article: glass sheet, area 155.15cm x 71.17cm, thickness 0.065 cm.
2) Soaking the glass product obtained in the step 1) in a chemical toughening agent, and taking out the glass product after toughening treatment to obtain a toughened glass product; wherein the toughening treatment temperature is 400 ℃, and the toughening treatment time is 300 min; the chemical toughening agent comprises the following components in percentage by mass:
Figure BDA0002610469500000101
3) soaking the toughened glass product prepared in the step 2) in an alkali treatment agent, taking out, and washing for 10min by using hydrochloric acid with the concentration of 10 wt% to prepare a glass intermediate; wherein the soaking temperature is 25 deg.C, and the soaking time is 60 min; the alkali treatment agent comprises the following components in percentage by mass:
Figure BDA0002610469500000102
4) soaking the glass intermediate obtained in the step 3) in an acid treatment agent, taking out, and washing for 10min by using a 10 wt% sodium hydroxide aqueous solution; obtaining a strengthened glass product; wherein the soaking temperature is 25 deg.C, and the soaking time is 60 min; the acid treatment agent comprises the following components in percentage by mass:
Figure BDA0002610469500000103
example 2
The method comprises the following specific steps.
1) Providing a glass article: glass sheet, area 155.15cm x 71.17cm, thickness 0.065 cm.
2) Soaking the glass product obtained in the step 1) in a chemical toughening agent, and taking out the glass product after toughening treatment to obtain a toughened glass product; wherein the toughening treatment temperature is 400 ℃, and the toughening treatment time is 300 min; the chemical toughening agent comprises the following components in percentage by mass:
Figure BDA0002610469500000104
Figure BDA0002610469500000111
3) soaking the toughened glass product prepared in the step 2) in an alkali treatment agent, taking out, and washing for 10min by using hydrochloric acid with the concentration of 10 wt% to prepare a glass intermediate; wherein the soaking temperature is 25 deg.C, and the soaking time is 60 min; the alkali treatment agent comprises the following components in percentage by mass:
Figure BDA0002610469500000112
4) soaking the glass intermediate obtained in the step 3) in an acid treatment agent, taking out, and washing for 10min by using a 10 wt% sodium hydroxide aqueous solution; obtaining a strengthened glass product; wherein the soaking temperature is 70 deg.C, and the soaking time is 60 min; the acid treatment agent comprises the following components in percentage by mass:
Figure BDA0002610469500000113
example 3
The method comprises the following specific steps.
1) Providing a glass article: glass sheet having an area of 155.15cm by 75.17cm and a thickness of 0.065 cm.
2) Soaking the glass product obtained in the step 1) in a chemical toughening agent, and taking out the glass product after toughening treatment to obtain a toughened glass product; wherein the toughening treatment temperature is 400 ℃, and the toughening treatment time is 300 min; the chemical toughening agent comprises the following components in percentage by mass:
Figure BDA0002610469500000114
3) soaking the toughened glass product obtained in the step 2) in an alkali treatment agent, taking out, and washing for 10min by using hydrochloric acid with the concentration of 10 wt% to obtain a glass intermediate; wherein the soaking temperature is 70 deg.C, and the soaking time is 60 min; the alkali treatment agent comprises the following components in percentage by mass:
Figure BDA0002610469500000121
4) soaking the glass intermediate obtained in the step 3) in an acid treatment agent, taking out, and washing for 10min by using a 10 wt% sodium hydroxide aqueous solution; obtaining a strengthened glass product; wherein the soaking temperature is 25 deg.C, and the soaking time is 60 min; the acid treatment agent comprises the following components in percentage by mass:
Figure BDA0002610469500000122
example 4
Example 4 is essentially the same as example 3, except that: the acid treatment agent used in step 4) in example 4 comprises the following components in percentage by mass:
Figure BDA0002610469500000123
comparative example 1
The method comprises the following specific steps.
1) Providing a glass article: glass sheet having an area of 155.15cm by 75.17cm and a thickness of 0.065 cm.
2) Soaking the glass product obtained in the step 1) in a chemical toughening agent, and taking out the glass product after toughening treatment to obtain a toughened glass product; wherein the toughening treatment temperature is 400 ℃, and the toughening treatment time is 300 min; the chemical toughening agent comprises the following components in percentage by mass:
Figure BDA0002610469500000124
Figure BDA0002610469500000131
3) soaking the toughened glass obtained in the step 2) in an acid treatment agent, taking out, and cleaning for 10min by using a 10 wt% sodium hydroxide aqueous solution; obtaining a strengthened glass intermediate; wherein the components of the acid treatment agent and the conditions of the acid treatment are the same as those of the acid treatment in step 4) in example 3.
4) Soaking the strengthened glass intermediate obtained in the step 3) in an alkali treatment agent, taking out, and washing with water until the washing liquor is neutral to obtain a glass intermediate; wherein the composition of the alkali treatment agent and the conditions of the alkali treatment are the same as those of the alkali treatment in step 3) in example 3.
Example 5
The reinforced glass articles prepared in examples 1-4 and comparative example 1 were subjected to the following performance tests:
1) the drop impact test formula was performed on the strengthened glass articles prepared in examples 1 to 4 and comparative example 1: reference standard: GB9962-1999, records the ball drop height at which the glassine product breaks, with higher ball drop height representing better impact resistance of the glassine product.
2) The static pressure test is performed on the strengthened glass products prepared in the embodiments 1-4 and the comparative example 1, specifically referring to the standard GB 2458-2009, the pressure borne by the glass product when it breaks is recorded, and the higher the pressure is, the better the pressure resistance of the glass product is. Specific results are shown in table 1.
TABLE 1
Group of Ball height (cm) Static pressure (N)
Example 1 135 2236.06
Example 2 145 2731.90
Example 3 160 3728.55
Example 4 115 1973.43
Comparative example 1 65 1649.57
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A method of making a strengthened glass article, comprising the steps of:
providing a glass article;
placing the glass product in a chemical toughening agent for toughening treatment to obtain a toughened glass product;
placing the toughened glass product in an alkali treatment agent for alkali treatment to prepare a toughened glass intermediate;
placing the strengthened glass intermediate into an acid treatment agent for acid treatment to obtain a strengthened glass product;
wherein the chemical toughening agent contains a potassium salt; the components of the acid treatment agent include a fluoride salt and an acidic agent, which is not hydrofluoric acid.
2. The method of making a strengthened glass article according to claim 1, wherein the acid treatment comprises the following components in mass percent:
1 to 20 percent of villiaumite;
5 to 10 percent of acid reagent;
0.05 to 5 percent of surfactant;
the balance being water.
3. The method of making a strengthened glass article according to claim 2, wherein the fluoride salt is selected from at least one of sodium fluoride, potassium fluoride, and ammonium fluoride; the acidic reagent is at least one of organic acid, sulfuric acid, nitric acid, hydrochloric acid and phosphoric acid; the surfactant is a cationic surfactant.
4. The method of making a strengthened glass article according to claim 1, wherein the acid treatment and/or the alkali treatment are under the following conditions: soaking at 20-90 deg.c for 20-240 min.
5. The method of making a strengthened glass article according to claim 4, wherein after the step of alkali treating and before the step of acid treating, further comprising the steps of:
and washing the strengthened glass intermediate by using acid, wherein the acid is at least one of organic acid and inorganic acid.
6. The method of making a strengthened glass article according to any one of claims 1 to 5, wherein the chemical toughening agent comprises the following components in weight percent:
Figure FDA0002610469490000011
7. the method of any of claims 1 to 5, wherein the tempering temperature is 350 ℃ to 470 ℃ and the tempering time is 100min to 500 min.
8. The method of making a strengthened glass article according to any one of claims 1 to 5, wherein the alkali treatment agent comprises the following components in mass percent:
10 to 30 percent of strong base;
0-10% of basic salt;
0-1% of a surfactant;
the balance being water.
9. The method of claim 8, wherein the strong base is selected from at least one of sodium hydroxide, potassium hydroxide, calcium hydroxide, and barium hydroxide; the basic salt is selected from at least one of basic carbonate, basic phosphate and basic silicate.
10. A strengthened glass product produced by the method for producing a strengthened glass according to any one of claims 1 to 9.
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