CN109928607B - Glass re-forming process - Google Patents
Glass re-forming process Download PDFInfo
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- CN109928607B CN109928607B CN201910342014.4A CN201910342014A CN109928607B CN 109928607 B CN109928607 B CN 109928607B CN 201910342014 A CN201910342014 A CN 201910342014A CN 109928607 B CN109928607 B CN 109928607B
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- 239000011521 glass Substances 0.000 title claims abstract description 214
- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000011248 coating agent Substances 0.000 claims abstract description 76
- 238000000576 coating method Methods 0.000 claims abstract description 76
- 238000010438 heat treatment Methods 0.000 claims abstract description 41
- 230000003287 optical effect Effects 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 23
- 238000000465 moulding Methods 0.000 claims abstract description 19
- 238000012545 processing Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 120
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 39
- 239000003973 paint Substances 0.000 claims description 36
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 27
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 27
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 27
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 26
- 235000019353 potassium silicate Nutrition 0.000 claims description 25
- 239000012459 cleaning agent Substances 0.000 claims description 21
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims description 19
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 18
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 18
- 235000011152 sodium sulphate Nutrition 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 15
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 13
- 244000060011 Cocos nucifera Species 0.000 claims description 13
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 13
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 13
- 238000000748 compression moulding Methods 0.000 claims description 13
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- -1 acyl sarcosinate Chemical compound 0.000 claims description 5
- 229940071089 sarcosinate Drugs 0.000 claims description 3
- 238000007496 glass forming Methods 0.000 abstract description 14
- 238000002425 crystallisation Methods 0.000 abstract description 12
- 230000008025 crystallization Effects 0.000 abstract description 12
- 230000007547 defect Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000000227 grinding Methods 0.000 abstract description 6
- 230000008602 contraction Effects 0.000 abstract description 5
- 239000005304 optical glass Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 28
- 238000003756 stirring Methods 0.000 description 23
- KSAVQLQVUXSOCR-UHFFFAOYSA-M sodium lauroyl sarcosinate Chemical compound [Na+].CCCCCCCCCCCC(=O)N(C)CC([O-])=O KSAVQLQVUXSOCR-UHFFFAOYSA-M 0.000 description 11
- 238000004031 devitrification Methods 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- 108700004121 sarkosyl Proteins 0.000 description 6
- 229940045885 sodium lauroyl sarcosinate Drugs 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 206010040925 Skin striae Diseases 0.000 description 4
- 239000005388 borosilicate glass Substances 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000007522 mineralic acids Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002667 nucleating agent Substances 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 230000002269 spontaneous effect Effects 0.000 description 3
- NLSFWPFWEPGCJJ-UHFFFAOYSA-N 2-methylprop-2-enoyloxysilicon Chemical compound CC(=C)C(=O)O[Si] NLSFWPFWEPGCJJ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000010425 asbestos Substances 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000005303 fluorophosphate glass Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000002407 reforming Methods 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- HJDITXMCJQRQLU-UHFFFAOYSA-N 2-[dodecanoyl(methyl)amino]acetate;tris(2-hydroxyethyl)azanium Chemical compound OCCN(CCO)CCO.CCCCCCCCCCCC(=O)N(C)CC(O)=O HJDITXMCJQRQLU-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
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- 238000001764 infiltration Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
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- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- 239000003960 organic solvent Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- JEMLSRUODAIULV-UHFFFAOYSA-M potassium;2-[dodecanoyl(methyl)amino]acetate Chemical compound [K+].CCCCCCCCCCCC(=O)N(C)CC([O-])=O JEMLSRUODAIULV-UHFFFAOYSA-M 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Landscapes
- Glass Compositions (AREA)
Abstract
The invention discloses a glass re-forming process. The process comprises the following steps: 1) cleaning; 2) drying; 3) coating; 4) softening and molding. The process can effectively inhibit the formation of defects such as crystallization, stripes, stones and the like in the glass forming process, and can effectively inhibit the phenomena of nonuniform glass bodies, shrinkage lines and the like caused by factors such as nonuniform heating, thermal expansion, cold contraction and the like, so that the prepared glass forming product has excellent optical characteristics and mechanical properties, achieves the expected value of an optical glass element, and avoids the waste of materials caused by the removal of nonuniform glass parts through grinding or grinding and the like in the deep processing process.
Description
Technical Field
The invention belongs to the technical field of glass processing, and particularly relates to a glass re-forming process.
Background
before the glass is further processed into an optical element, it is often necessary to form a glass molded product having a shape similar to that of the optical element from a glass raw material, and then grind, polish, and finish the glass into the optical element. The glass reforming process, which is a method for manufacturing a glass molded article, includes the steps of: the glass raw material is cut into glass blanks meeting certain weight requirements, the glass blanks are heated to be softened, and various glass forming products meeting the design weight and shape requirements are formed and used for glass deep processing. The quality of the glass shaped article is directly related to the quality of the final optical device product. Defects such as stones, striae, devitrification, etc. generated during the glass reshaping process affect the refraction and reflection of the glass, and affect the desired optical, thermal and mechanical properties of the optical element.
The molding viscosity range of the glass is 103～106.6As, viscosity of devitrification of glass is 103～108as the crystallization viscosity and temperature range of the glass are respectively in the corresponding glass forming viscosity and temperature range, crystallization has already occurred in the glass forming process. When the glass is kept in a temperature condition favorable for crystal formation and growth for a long time, the chemical composition unevenness in the glass is a main factor for promoting devitrification of the glass body. Devitrified stones often first appear at the boundaries of the phases, such as on the surface of the glass, near the bubbles, and in streaks. When a glass gob of glass which is easily crystallized is heated to a temperature at which press molding can be performed, the surface of the glass gob is often hardened by crystallization, and when a glass gob having a hardened coating film formed by crystallization of the surface is molded, the hardened coating film is mixed into the inside of the glass gob, so that the resulting glass molded article becomes uneven from the surface to a deep portion. In such an uneven glass molded article, it is necessary to remove uneven portions such as a hardened coating mixed therein by grinding, polishing, or the like. As a result, the material loss increases, which causes a problem of an increase in manufacturing cost.
Calculus refers to inherent defects in glass and is divided into raw material calculus, devitrified calculus and the like. The impurities introduced into the glass, as well as particles, dust, or other particles in the air during the forming process, or machine debris and impurities (e.g., iron flakes, steel slag, etc.) introduced during the processing process, can induce the formation of non-spontaneous nucleation crystals in the glass in the form of nucleating agents, and can also or alternatively generate black stones or bubbles on the glass sheet. In addition, the crystals of the surface-crystallized glass are re-dissolved at a higher temperature, so that the surface of the glass is easily streaked. Therefore, the factors inducing defects such as stones, striae, devitrification, etc. generated in the glass forming process are mutually influenced. The quality of glass formed is closely related to the forming process, and the above defects are expected to be overcome by optimizing the steps of the forming process, adjusting production parameters or taking corresponding measures. Chinese patent application publication No. CN 105837050a discloses a glass re-molding process, which comprises the following steps: 1) coating the surface of the glass blank by using a coating; 2) placing the coated glass blank on a porcelain box, conveying the glass blank into a heating area in a softening furnace through a conveying device, and heating the glass blank in a sectional and staged manner to soften the glass blank; 3) placing the softened glass blank in a forming die for compression molding; 4) and (4) removing the coating layer on the surface after the glass is molded, cooled and demoulded to obtain the glass preform. The process can effectively inhibit the phenomena of nonuniform glass body, shrinkage wrinkles and the like caused by nonuniform heating, expansion with heat and contraction with cold and other factors. However, the process does not consider whether the defect of glass crystallization is overcome, meanwhile, the coating is composed of asbestos powder, organic silicon modified acrylate resin, methacryloxy silane, aluminosilicate and a low-boiling-point organic solvent, the boiling point of the methacryloxy silane is low and easy to lose at the forming temperature range of 400-800 ℃, so that the coating is unstable, and the asbestos powder is high-temperature resistant, exists on the surface of the glass in a solid form and is easy to serve as a nucleating agent to induce the generation of non-spontaneous nucleation crystals in the glass.
Disclosure of Invention
The invention aims to provide a glass reshaping process. The process can effectively inhibit the formation of defects such as crystallization, stripes, stones and the like in the glass forming process, and can effectively inhibit the phenomena of nonuniform glass bodies, shrinkage lines and the like caused by factors such as nonuniform heating, thermal expansion, cold contraction and the like, so that the prepared glass forming product has excellent optical characteristics and mechanical properties, reaches the expected value of an optical glass element, and avoids the waste of materials caused by the removal of nonuniform glass parts through grinding or grinding and the like in the deep processing process.
The invention is realized by the following technical scheme:
It is a first object of the present invention to provide a glass reshaping process comprising the steps of:
(1) Cleaning: washing the glass blank with clear water for 2-3 times, then soaking the glass blank in a water-based glass cleaning agent for ultrasonic treatment for 30-45 min, and then washing the glass blank with clear water for 2-3 times;
(2) Drying: drying the cleaned glass blank at 55-65 ℃, and cooling for later use;
(3) Coating: coating the water-based paint on a glass blank, and drying at 80-100 ℃ to obtain a glass coating;
(4) Softening and molding: heating and softening the glass coating, and performing compression molding to obtain a glass molding product.
The water-based paint of the step (3) comprises the following components in percentage by mass: 40-50% of water glass, 5-15% of sodium hexametaphosphate, 5-15% of potassium pyrophosphate, 5-10% of sodium sulfate and 25-35% of water.
the coating thickness of the water-based coating in the step (3) on the glass blank is 10-100 mu m.
Preferably, the coating thickness of the water-based paint in the step (3) on the glass blank is 10-50 μm.
The heating and softening of the glass coating in the step (4) is specifically as follows: and (3) putting the glass coating into a heat treatment furnace, and carrying out staged heating treatment for 10-15 min at 600-1200 ℃ to soften the glass coating.
the stage type heating treatment specifically comprises the following steps: firstly, treating at 600-700 ℃ for 3-5 min, then treating at 800-900 ℃ for 4-6 min, and then treating at 1000-1200 ℃ for 3-4 min.
The water-based glass cleaning agent comprises the following components in percentage by mass: 5-8% of acyl sarcosinate, 2-4% of coconut diethanolamide, 3-5% of potassium hydroxide, 2-4% of disodium ethylene diamine tetraacetate and the balance of water.
The acyl sarcosinate salt includes but is not limited to sodium lauroyl sarcosinate, potassium lauroyl sarcosinate, and TEA lauroyl sarcosinate.
the frequency of the ultrasonic treatment in the step (1) is 45-55 Hz.
It is a second object of the present invention to provide a glass shaped article which is produced by the above glass reshaping process.
The third object of the present invention is to provide an optical element prepared by deep processing the above glass molded article.
the deep processing comprises the step of removing the coating of the water-based paint of the glass forming product.
The device for testing the glass reshaping process comprises a softening furnace, a control device and a porcelain box, wherein a glass blank inlet and a glass blank outlet are arranged on a furnace body of the softening furnace, a glass blank conveying device is arranged in the furnace body, a heating chamber in the furnace body is divided into three areas, namely a 600-700 ℃ heating area, a 800-900 ℃ heating area and a 1000-1200 ℃ heating area, and a silicon carbide rod resistor with a ceramic core is arranged in each heating area for radiation heat transfer. The furnace body is matched with the radiation heat transfer tubes of the silicon carbide rod resistors in the furnace body, and a corresponding power supply cable is arranged outside the furnace body and is connected with a control device so as to control the work of each heating area.
The glass reshaping process comprises the steps of 1) cleaning; 2) drying; 3) coating; 4) softening, molding and the like. The glass blank is cleaned by using a water-based glass cleaning agent before coating, and oil stain, dust, oxide and the like on the surface of the glass are sufficiently removed by utilizing the saponification capacity of potassium hydroxide in the glass cleaning agent, the washing, emulsifying, permeating, solubilizing and foaming characteristics of acyl sarcosinate and coconut diethanolamide and the metal ion complexing action of disodium ethylene diamine tetraacetate, so that the impurities are prevented from existing on the surface of the glass in a solid form in a glass forming process and being used as a nucleating agent to induce the generation of non-spontaneous nucleation crystals in the glass.
The invention adopts water-based paint to coat the cleaned, dried and cooled glass blank, adopts a staged heating treatment mode to soften the glass, utilizes the gradient increasing melting temperature of sodium hexametaphosphate, sodium sulfate, potassium pyrophosphate and water glass to adapt to a staged heating softening process, leads the glass surface to contain molten inorganic acid salt solution in different softening periods, and inhibits the crystallization phenomenon of the glass surface through the infiltration of the inorganic acid salt solution. In addition, in the high-temperature stage, the water glass releases a large amount of water vapor and is foamed and cured, Si-O tetrahedrons in the water glass are polymerized to form a Si-O-Si net-shaped coating, the sodium hexametaphosphate and the potassium pyrophosphate have strong complexing capability and have good fixing effect on alkali metal ions in the water glass, the curing of the water-based coating is promoted, the coating formed after the curing has good compressive strength and heat insulation performance, and the phenomena that the glass body is uneven and shrinkage lines are generated due to factors such as uneven heating of the surface and the inside of the glass, thermal expansion and cold contraction and the like in the softening stage of the glass are avoided.
compared with the prior art, the invention has the following beneficial effects:
(1) the glass re-forming process can effectively inhibit the formation of defects such as crystallization, stripes, stones and the like in the glass forming process, and can effectively inhibit the phenomena of nonuniform glass bodies, shrinkage lines and the like caused by factors such as nonuniform heating, expansion with heat and contraction with cold and the like, so that the prepared glass forming product has excellent optical characteristics and mechanical properties, achieves the expected value of an optical glass element, and avoids the waste of materials caused by the removal of nonuniform glass parts through grinding or lapping and the like in the deep processing process.
(2) The water-based glass cleaning agent and the water-based paint used in the invention can not damage the surface of the glass blank, the compatibility with the glass is better, the composition of the water-based paint is adapted to the softening temperature, the formed coating layer can not only generate the heat preservation effect in the heating process, but also can inhibit the crystallization by gradually forming the inorganic acid salt solution.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to be limiting thereof.
the water glass in the following examples is a sodium silicate aqueous solution having a concentration of 1.35 to 1.50 g/mL.
The commercially available broken optical glass pieces are used as glass blanks for preparing glass forming products, and the refractive index and the softening point of the broken optical glass pieces are shown in the following table 1:
TABLE 1 Property parameters of different glass blanks
Example 1
a glass reshaping process comprising the steps of:
(1) Cleaning: washing the fluorophosphate glass block with clear water for 2 times, then soaking in a water-based glass cleaning agent for ultrasonic treatment for 30min, and then washing with clear water for 3 times;
(2) Drying: drying the cleaned fluorophosphate glass block at 60 ℃, and cooling for later use;
(3) Coating: coating the water-based paint on a glass blank with the coating thickness of 50 mu m, and drying at 90 ℃ to obtain a glass coating;
(4) softening and molding: putting the glass coating in a heat treatment furnace, and performing staged heating softening treatment at 600-1200 ℃ for 12min, specifically treating at 600-700 ℃ for 4min, then treating at 800-900 ℃ for 5min, and then treating at 1000-1200 ℃ for 3 min; and (3) introducing the softened glass coating into a compression molding die, performing compression molding, and demolding to obtain a glass molded product.
The water-based glass cleaning agent comprises the following components in percentage by mass: 7% of sodium lauroyl sarcosinate, 3% of coconut diethanolamide, 4% of potassium hydroxide, 3% of disodium ethylene diamine tetraacetate and the balance of water. Preparation: adding sodium lauroyl sarcosine, coconut diethanolamide, potassium hydroxide and disodium ethylene diamine tetraacetate into water, and stirring to dissolve to obtain the water-based glass cleaning agent.
The water-based paint comprises the following components in percentage by mass: 40% of water glass, 15% of sodium hexametaphosphate, 10% of potassium pyrophosphate, 5% of sodium sulfate and 30% of water. Preparation: adding sodium hexametaphosphate, potassium pyrophosphate and sodium sulfate into water, stirring to dissolve, then adding water glass, and uniformly stirring to obtain the water-based paint.
example 2
a glass reshaping process comprising the steps of:
(1) cleaning: washing borosilicate glass blocks with clear water for 2 times, then soaking the borosilicate glass blocks in a water-based glass cleaning agent for ultrasonic treatment for 30min, and then washing the borosilicate glass blocks with clear water for 3 times;
(2) drying: drying the cleaned borosilicate glass block at 55 ℃, and cooling for later use;
(3) Coating: coating the water-based paint on a glass blank with the coating thickness of 100 mu m, and drying at 100 ℃ to obtain a glass coating;
(4) Softening and molding: putting the glass coating in a heat treatment furnace, and performing staged heating softening treatment at 600-1200 ℃ for 15min, specifically treating at 600-700 ℃ for 5min, then treating at 800-900 ℃ for 6min, and then treating at 1000-1200 ℃ for 4 min; and (3) introducing the softened glass coating into a compression molding die, performing compression molding, and demolding to obtain a glass molded product.
The water-based glass cleaning agent comprises the following components in percentage by mass: 8% of sodium lauroyl sarcosinate, 2% of coconut diethanolamide, 5% of potassium hydroxide, 2% of disodium ethylene diamine tetraacetate and the balance of water. Preparation: adding sodium lauroyl sarcosine, coconut diethanolamide, potassium hydroxide and disodium ethylene diamine tetraacetate into water, and stirring to dissolve to obtain the water-based glass cleaning agent.
The water-based paint comprises the following components in percentage by mass: 50% of water glass, 15% of sodium hexametaphosphate, 5% of potassium pyrophosphate, 5% of sodium sulfate and 25% of water. Preparation: adding sodium hexametaphosphate, potassium pyrophosphate and sodium sulfate into water, stirring to dissolve, then adding water glass, and uniformly stirring to obtain the water-based paint.
Example 3
A glass reshaping process comprising the steps of:
(1) Cleaning: washing the H-K9L glass block with clear water for 3 times, then soaking in a water-based glass cleaning agent for ultrasonic treatment for 45min, and then washing with clear water for 2 times;
(2) Drying: drying the cleaned H-K9L glass block at 65 ℃, and cooling for later use;
(3) Coating: coating the water-based paint on a glass blank with the coating thickness of 10 mu m, and drying at 80 ℃ to obtain a glass coating;
(4) Softening and molding: putting the glass coating in a heat treatment furnace, and performing staged heating softening treatment at 600-1200 ℃ for 10min, specifically treating at 600-700 ℃ for 3min, then treating at 800-900 ℃ for 4min, and then treating at 1000-1200 ℃ for 3 min; and (3) introducing the softened glass coating into a compression molding die, performing compression molding, and demolding to obtain a glass molded product.
the water-based glass cleaning agent comprises the following components in percentage by mass: 5% of sodium lauroyl sarcosinate, 4% of coconut diethanolamide, 3% of potassium hydroxide, 4% of disodium ethylene diamine tetraacetate and the balance of water. Preparation: adding sodium lauroyl sarcosine, coconut diethanolamide, potassium hydroxide and disodium ethylene diamine tetraacetate into water, and stirring to dissolve to obtain the water-based glass cleaning agent.
the water-based paint comprises the following components in percentage by mass: 40% of water glass, 5% of sodium hexametaphosphate, 15% of potassium pyrophosphate, 5% of sodium sulfate and 35% of water. Preparation: adding sodium hexametaphosphate, potassium pyrophosphate and sodium sulfate into water, stirring to dissolve, then adding water glass, and uniformly stirring to obtain the water-based paint.
Example 4
A glass reshaping process comprising the steps of:
(1) Cleaning: washing the B270 glass block with clear water for 3 times, then soaking in a water-based glass cleaning agent for ultrasonic treatment for 40min, and then washing with clear water for 3 times;
(2) Drying: drying the cleaned B270 glass block at 60 ℃, and cooling for later use;
(3) Coating: coating the water-based paint on a glass blank with the coating thickness of 30 mu m, and drying at 80 ℃ to obtain a glass coating;
(4) Softening and molding: putting the glass coating in a heat treatment furnace, and performing staged heating softening treatment at 600-1200 ℃ for 11min, specifically treating at 600-700 ℃ for 4min, then treating at 800-900 ℃ for 4min, and then treating at 1000-1200 ℃ for 3 min; and (3) introducing the softened glass coating into a compression molding die, performing compression molding, and demolding to obtain a glass molded product.
The water-based glass cleaning agent comprises the following components in percentage by mass: 6% of sodium lauroyl sarcosinate, 4% of coconut diethanolamide, 4% of potassium hydroxide, 3% of disodium ethylene diamine tetraacetate and the balance of water. Preparation: adding sodium lauroyl sarcosine, coconut diethanolamide, potassium hydroxide and disodium ethylene diamine tetraacetate into water, and stirring to dissolve to obtain the water-based glass cleaning agent.
the water-based paint comprises the following components in percentage by mass: 50% of water glass, 10% of sodium hexametaphosphate, 5% of potassium pyrophosphate, 10% of sodium sulfate and 25% of water. Preparation: adding sodium hexametaphosphate, potassium pyrophosphate and sodium sulfate into water, stirring to dissolve, then adding water glass, and uniformly stirring to obtain the water-based paint.
Example 5
A glass reshaping process comprising the steps of:
(1) Cleaning: mixing ZBeF6washing the glass block with clear water for 3 times, soaking in water-based glass cleaning agent, performing ultrasonic treatment for 35min, and washing with clear water for 3 times;
(2) Drying: the cleaned ZBeF6Drying the glass blocks at 65 ℃ and cooling for later use;
(3) coating: coating the water-based paint on a glass blank with the coating thickness of 50 mu m, and drying at 80 ℃ to obtain a glass coating;
(4) softening and molding: putting the glass coating in a heat treatment furnace, and performing staged heating softening treatment at 600-1200 ℃ for 10min, specifically treating at 600-700 ℃ for 3min, then treating at 800-900 ℃ for 4min, and then treating at 1000-1200 ℃ for 3 min; and (3) introducing the softened glass coating into a compression molding die, performing compression molding, and demolding to obtain a glass molded product.
the water-based glass cleaning agent comprises the following components in percentage by mass: 6% of sodium lauroyl sarcosinate, 2% of coconut diethanolamide, 5% of potassium hydroxide, 2% of disodium ethylene diamine tetraacetate and the balance of water. Preparation: adding sodium lauroyl sarcosine, coconut diethanolamide, potassium hydroxide and disodium ethylene diamine tetraacetate into water, and stirring to dissolve to obtain the water-based glass cleaning agent.
The water-based paint comprises the following components in percentage by mass: 45% of water glass, 10% of sodium hexametaphosphate, 5% of potassium pyrophosphate, 10% of sodium sulfate and 30% of water. Preparation: adding sodium hexametaphosphate, potassium pyrophosphate and sodium sulfate into water, stirring to dissolve, then adding water glass, and uniformly stirring to obtain the water-based paint.
Comparative example 1
The glass reshaping process of comparative example 1 was compared to example 1 except that the water-based coating used contained no water glass, and the glass was formed from sodium hexametaphosphate: potassium pyrophosphate: sodium sulfate: the water-based paint is prepared from the following components in a mass ratio of 5:5:3: 87: adding sodium hexametaphosphate, potassium pyrophosphate and sodium sulfate into water, and stirring to dissolve to obtain the water-based paint. The remaining steps and parameter conditions were the same as in example 1.
comparative example 2
the difference between the glass reshaping process of comparative example 2 and example 1 is that the water-based coating used is a 13% by mass aqueous solution of sodium hexametaphosphate (prepared by adding sodium hexametaphosphate to water and stirring to dissolve the sodium hexametaphosphate to obtain the water-based coating), and the water-based coating is heated by a heating zone at 600-700 ℃ for 12min, and the rest of the steps and parameter conditions are the same as those of example 1.
Comparative example 3
The glass reshaping process of comparative example 3 was compared to example 1, except that the water-based coating used was composed of water glass: sodium hexametaphosphate: the water-based paint is prepared from the following components in a mass ratio of 9:2: 6: adding sodium hexametaphosphate into water, stirring to dissolve, then adding water glass, and uniformly stirring to obtain a water-based coating; and heating by adopting a heating zone, namely treating at the temperature of 1000-1200 ℃ for 12min, wherein the rest steps and parameter conditions are the same as those of the embodiment 1.
comparative example 4
The glass reshaping process of comparative example 4 was compared to example 1, except that the water-based coating used was composed of water glass: sodium hexametaphosphate: sodium sulfate: the water-based paint is prepared from water with a mass ratio of 45:10:6:30 as follows: adding sodium hexametaphosphate and sodium sulfate into water, stirring to dissolve, then adding water glass, and uniformly stirring to obtain the water-based paint. The remaining steps and parameter conditions were the same as in example 1.
Comparative example 5
The glass reshaping process of comparative example 5 was compared to example 1, except that the water-based coating used was composed of water glass: sodium hexametaphosphate: potassium pyrophosphate: the water-based paint is prepared from the following components in a mass ratio of 9:2:2: 6: adding sodium hexametaphosphate and potassium pyrophosphate into water, stirring to dissolve, then adding water glass, and uniformly stirring to obtain the water-based paint. The remaining steps and parameter conditions were the same as in example 1.
Comparative example 6
The difference between the glass reforming process of comparative example 6 and example 1 is that the glass material was softened and formed without being coated with a water-based paint. The remaining steps and parameter conditions were the same as in example 1.
The surface observation of the glass shaped articles obtained in examples 1 to 5 and comparative examples 1 to 6 was carried out, and the appearance of devitrification, striae, and blisters of the above glass shaped articles was evaluated, and the results are shown in Table 2 below.
TABLE 2 quality evaluation of various glass moldings
the results showed that the glass shaped articles obtained in examples 1 to 5 exhibited no crystallization (non-devitrification) on the surface and no visible streaks of 100cm3Bubbles (diameter) contained in glass) The total sectional area is less than or equal to 0.003-0.03 mm2The invention can effectively inhibit the generation of devitrification, stripes and bubbles in the glass forming process. As can be seen from comparative examples 1 to 5, the adjustment of the composition of the water-based coating for glass and the softening step did not affect the devitrification of the glass but affected the formation of striae and blisters on the glass. Comparative example 6 shows that the glass material was softened and molded without being coated with the water-based paint, and that crystallization occurred(devitrification) and obvious parallel stripes and larger bubble cross-sectional area are also shown, which shows that the water-based coating has an important function of inhibiting the generation of devitrification, stripes and bubbles in the process of reshaping the glass blank.
further, the water-based coating layers of the glass shaped articles obtained in examples 1 to 5 and comparative examples 1 to 6 were removed, and the optical uniformity of the glass shaped articles was examined by the test method specified in GB/T7962.4, and the results are shown in Table 3.
TABLE 3 results of optical uniformity measurements on various glass moldings
| Group of | Δnmax | Rank of |
| Example 1 | ±2×10-6 | H1 |
| Example 2 | ±2×10-6 | H1 |
| Example 3 | ±2×10-6 | H1 |
| Example 4 | ±2×10-6 | H1 |
| Example 5 | ±2×10-6 | H1 |
| Comparative example 1 | ±10×10-6 | H3 |
| comparative example 2 | ±10×10-6 | H3 |
| Comparative example 3 | ±10×10-6 | H3 |
| Comparative example 4 | ±5×10-6 | H2 |
| Comparative example 5 | ±5×10-6 | H2 |
| Comparative example 6 | ±20×10-6 | H4 |
Note: Δ nmaxRefers to the maximum value of refractive index deviation of each part in the glass.
As a result, the glass moldings obtained in examples 1 to 5 had good optical uniformity, and the maximum value of the refractive index deviation Deltan at each portion in the glassmaxWithin + -2 × 10-6Within the range, the grade was H1, which is superior to the glass shaped articles obtained in comparative examples 1 to 6. From comparative examples 1 to 3, the water-based coating compositions do not containWater glass, or a water-based coating containing only sodium hexametaphosphate and heated by one heating zone, or a water-based coating containing only sodium hexametaphosphate and water glass and heated by one heating zone, may reduce the optical uniformity of the glass molded article. As can be seen from comparative examples 4 to 5, the absence of potassium pyrophosphate or sodium sulfate in the water-based paint also affects the optical uniformity of the glass shaped article. Comparative example 6 shows that the glass material was directly softened and molded without being coated with a water-based paint, and the optical uniformity of the glass molded article was significantly reduced.
Further, the water-based coating layers of the glass shaped articles obtained in examples 1 to 5 and comparative examples 1 to 6 were removed, and the glass shaped articles were subjected to middle and edge stress birefringence measurements in accordance with the test methods specified in GB/T7962.5-6, and the results are shown in Table 4.
TABLE 4 detection results of middle and edge stress birefringence of different glass moldings
Note: the middle optical path difference delta refers to the optical path difference of the middle part of the longest side of the glass in unit length; the edge optical path difference delta refers to the optical path difference per unit thickness at a position 5% of the diameter or side length of the glass from the edge.
The results show that the glass shaped articles obtained in examples 1 to 5 have smaller central and peripheral optical path difference δ, which are respectively 1 and S1, and are superior to those obtained in comparative examples 1 to 6, indicating that the glass shaped articles obtained by the glass reshaping process of the present invention have better mechanical stress, so that the anisotropy and non-uniformity of the optical properties of the glass under the influence of external mechanical load are reduced.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (7)
1. A glass reshaping process is characterized by comprising the following steps:
(1) cleaning: washing the glass blank with clear water for 2-3 times, then soaking the glass blank in a water-based glass cleaning agent for ultrasonic treatment for 30-45 min, and then washing the glass blank with clear water for 2-3 times;
(2) Drying: drying the cleaned glass blank at 55-65 ℃, and cooling for later use;
(3) Coating: coating the water-based paint on a glass blank, and drying at 80-100 ℃ to obtain a glass coating;
(4) Softening and molding: heating and softening the glass coating, and carrying out compression molding to obtain a glass molding product;
The water-based paint of the step (3) comprises the following components in percentage by mass: 40-50% of water glass, 5-15% of sodium hexametaphosphate, 5-15% of potassium pyrophosphate, 5-10% of sodium sulfate and 25-35% of water;
The heating and softening of the glass coating in the step (4) is specifically as follows: putting the glass coating in a heat treatment furnace, and carrying out staged heating treatment for 10-15 min at 600-1200 ℃ to soften the glass coating;
The stage type heating treatment specifically comprises the following steps: firstly, treating at 600-700 ℃ for 3-5 min, then treating at 800-900 ℃ for 4-6 min, and then treating at 1000-1200 ℃ for 3-4 min.
2. the glass reshaping process of claim 1, wherein the coating thickness of the water-based coating in the step (3) on the glass blank is 10-100 μm.
3. The glass reshaping process of claim 1, wherein the water-based glass cleaner comprises the following components in percentage by mass: 5-8% of acyl sarcosinate, 2-4% of coconut diethanolamide, 3-5% of potassium hydroxide, 2-4% of disodium ethylene diamine tetraacetate and the balance of water.
4. The glass reshaping process of claim 1, wherein the frequency of the ultrasonic treatment of step (1) is 45-55 Hz.
5. A glass molded article characterized by being produced by the glass reshaping process according to any one of claims 1 to 4.
6. an optical element produced by deep processing the glass molding according to claim 5.
7. An optical element as recited in claim 6, wherein said further processing comprises the step of removing a coating of the water-based paint from the glass shaped article.
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|---|---|---|---|---|
| CN104470861A (en) * | 2012-07-18 | 2015-03-25 | Hoya株式会社 | Glass molded article and method for producing same, optical element blank, and optical element and method for producing same |
| CN105837050A (en) * | 2016-03-25 | 2016-08-10 | 蔡丝英 | Glass re-shaping process |
| CN106544195A (en) * | 2016-10-07 | 2017-03-29 | 常州市鼎日环保科技有限公司 | A kind of preparation method of automobile glass cleaning agent |
| CN106753873A (en) * | 2017-01-13 | 2017-05-31 | 蓝思科技（长沙）有限公司 | A kind of glass cleaner and its application method |
| CN107057878A (en) * | 2017-04-19 | 2017-08-18 | 中南大学 | A kind of environment-friendly type cleaning agent for optical glass and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104470861A (en) * | 2012-07-18 | 2015-03-25 | Hoya株式会社 | Glass molded article and method for producing same, optical element blank, and optical element and method for producing same |
| CN105837050A (en) * | 2016-03-25 | 2016-08-10 | 蔡丝英 | Glass re-shaping process |
| CN106544195A (en) * | 2016-10-07 | 2017-03-29 | 常州市鼎日环保科技有限公司 | A kind of preparation method of automobile glass cleaning agent |
| CN106753873A (en) * | 2017-01-13 | 2017-05-31 | 蓝思科技（长沙）有限公司 | A kind of glass cleaner and its application method |
| CN107057878A (en) * | 2017-04-19 | 2017-08-18 | 中南大学 | A kind of environment-friendly type cleaning agent for optical glass and preparation method thereof |
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