CN1044448A - Surface strengthening method for optical glass elements and high-strength products thereof - Google Patents

Surface strengthening method for optical glass elements and high-strength products thereof Download PDF

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Publication number
CN1044448A
CN1044448A CN 90105773 CN90105773A CN1044448A CN 1044448 A CN1044448 A CN 1044448A CN 90105773 CN90105773 CN 90105773 CN 90105773 A CN90105773 A CN 90105773A CN 1044448 A CN1044448 A CN 1044448A
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China
Prior art keywords
optical glass
ion
glass elements
exchange
early stage
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CN 90105773
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Chinese (zh)
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孙玉珍
郭晓
苏友安
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Institute of Optics and Electronics of CAS
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Institute of Optics and Electronics of CAS
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Priority to CN 90105773 priority Critical patent/CN1044448A/en
Publication of CN1044448A publication Critical patent/CN1044448A/en
Pending legal-status Critical Current

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Abstract

Surface strengthening method for optical glass elements and high-strength products thereof relate to the surface reinforcing method of thin-walled, special-shaped optical glass device.Be applicable to the intensity that strengthens various thin-walleds, special-shaped optical glass elements face.It is characterized in that adopting surface chemistry pre-treatment in early stage and ion-exchange heat treatment phase bonded process for over-all strengthening, determine rational solution, molten salt bath prescription and processing parameter, thereby can make high strength optics glass elements.

Description

Surface strengthening method for optical glass elements and high-strength products thereof
The present invention is a kind of surface strengthening method for optical glass elements and high-strength products thereof, relates to the surface reinforcing method of thin-wall special-shaped optical glass device.It comprises the step of ion-exchange surface enhancement method, is applicable to the intensity that strengthens various thin-wall special-shaped optical glass elements faces.
Optical glass device is a kind of intensely processed products, requires to have accurate dimension and good smooth finish and certain optical characteristics.But general thin-wall special-shaped optical glass device, fragility is big, intensity is low, frangible, use dangerous, cause waste easily.For this reason, adopt various Enhancement Method to improve the intensity of glass elements, existing both at home and abroad certain research, disclosing a kind of employing ion-exchange surface enhancement method as United States Patent (USP) UPS4036623 increases its intensity, thereby makes the glass mirror less than 2 millimeters.But according to the Z-80 test method, its intensity is lower, can only resist 0.56 ounce (about 16 grams) bearing steel ball from 50 inches (about 1.27 meters) free-falling surging forces of eminence, and this simple ion-exchange surface enhancement method, be only applicable to strengthen the glass elements of soda-lime-silica glass system, the scope of application is very little, thereby has limited the utilization of making high strength optics glass elements products material greatly.Another kind is to adopt the chemical surface treatment technology that the optical glass device that titanium system, boron system, calcium are is carried out intensive treatment, but because silicone content is low, its surface easily produces defectives such as burn into cut, fluffing again, reduce surface quality thus, very easily cause waste product to produce, can't in actual industrial production, use.The somebody once managed to adopt the physical surface enhancement method, only was applicable in this way to make thickness greater than 3 millimeters glass protecting eyeglass.This eyeglass also has slight deformation, changes its optical characteristics easily, but also can not adopt ordinary skill cutting, edging, and processing is difficulty relatively, thereby also is difficult to industrial actual applying.
The objective of the invention is to avoid above-mentioned deficiency of the prior art and a kind of surface strengthening method for optical glass elements new, applied widely is provided; and the high strength optics glass elements that thickness is little, intensity is high that utilizes this method to make, as the high strength protection eyeglass of various opticinstruments, all kinds of high strength optics glass eye eyeglasses etc.
Purpose of the present invention can reach by following measure: the process for over-all strengthening that adopts chemical conversion treatment to combine with the ion-exchange surface reinforcement, the optical glass device that will contain alkali silicate glass system carries out earlier surface chemistry pre-treatment in early stage in mixed chemical solution, after cleaning, drying, preheating, put into the fused salt mixt bath and carry out ion-exchange thermal treatment, take out then and after Xu Leng, cleaning, drying, can make high strength optics glass elements product.
Purpose of the present invention can also reach by following measure: mixed chemical solution is a kind of aqueous solution that contains sulfuric acid and salt, and its pH value is 2~6.Surface chemistry pretreatment time in early stage (under the normal temperature) is 0.5~5 hour.The component that fused salt mixt during ion-exchange thermal treatment is bathed is: KNO 390~98WT%, H 2SlO 30.5~5WT%, KOH 0~1.5WT%; KAl(SO 4) 20.8~2WT%, K 2CO 30.4~1.5WT%, ZrO 20.3~2WT%.Its heat treatment time is 5~20 hours, and thermal treatment temp is lower than the softening temperature of glass elements, is 350 ℃~500 ℃.
Description of drawings:
Fig. 1: process flow sheet of the present invention
Fig. 2: heating furnace structure figure
Among Fig. 1: (1) optical glass device (2) chemical conversion treatment in early stage
(3) cleaning, dry (4) preheating
(5) ion-exchange thermal treatment (6) Xu Leng that comes out of the stove
(7) cleaning, dry (8) test package
(9) product
Among Fig. 2: 1, optical glass lens 2, anchor clamps
3, molten salt bath 4, dissolved salt groove
5, heat source body 6, oven wall
7, heating furnace cover 8, thermopair
The present invention does a step below in conjunction with embodiment and describes in detail:
Example one: accurately machined optical glass lens, its glass system is for containing the alkali silicate glass system, and its center thickness is less than 2 millimeters, and diameter is 60 millimeters.At room temperature, it is that 3 mixed chemical solution carries out surface chemistry pre-treatment in early stage that optical glass lens is put into pH value, and the treatment time is 1 hour, and the component of its solution is: H 2SO 410WT%; K 2SO 43.5WT%; N 2SO 43.5WT%; H 2O 83WT%.To take out through pretreated eyeglass, with clear water clean, dry, it is preheated to 400 ℃ again.Be incubated after 1 hour and take out, put into the process furnace (as shown in Figure 2) that the fused salt mixt bath is housed again and carry out ion-exchange thermal treatment, its thermal treatment temp is controlled at below the softening temperature of glass mirror, and promptly 500 ℃ ± 5 ℃, heat treatment time is 6 hours.The component of mixing the dissolved salt bath is: KNO 395WT%, H 2SlO 32WT%, KOH 1WT%, KAl(SO 4) 21WT%, K 2CO 30.5WT%, ZrO 20.5WT%.To after taking out Xu Leng, cleaning, drying, the eyeglass after the ion-exchange thermal treatment can obtain high-intensity optical glass lens.
Example two: accurately machined, contain the optical glass lens of alkali silicate glass system, the certain curvature radius is arranged, its center thickness is less than 1 millimeter, and diameter is 70 millimeters.At room temperature, it is 5 mixed chemical solution that eyeglass is put into pH value, carries out surface chemistry pre-treatment in early stage, and the treatment time is 1.5 hours, and its solution component is: H 2SO 412WT%, K 2SO 44.2WT%, Na 2SO 44.2WT%, H 2O 79WT%.To take out through pretreated eyeglass, with clear water clean, dry, it is preheated to 400 ℃ again, be incubated after 1 hour and take out, put into the process furnace that the fused salt mixt bath is housed again and carry out ion-exchange thermal treatment, its thermal treatment temp is 450 ℃ ± 5 ℃, its heat treatment time is 12 hours, and the component that fused salt mixt is bathed is: KNO 395WT%, H 2SiO 31.5WT%, KOH 0.4WT%, KAl(SO 4) 21.5WT%, K 2CO 30.6WT%, ZrO 21.0WT%.To after taking out Xu Leng, cleaning, drying, the eyeglass after the ion-exchange thermal treatment can obtain high-intensity optical glass lens.Its intensity can resist the surging force of the heavy bearing steel ball of 100~130g from 1.3 meters high free-fallings; Its Vickers' hardness is when loading 100g, by original 872.8Kg/mm 2, bring up to 1116.6Kg/mm 2; Its bending strength is by original 6.73Kg/mm 2Bring up to 24.38Kg/mm 2; In 90 ℃ ± 1 ℃ water, corroded 64 hours its optical glass lens original weightless 2.1 * 10 -2G/cm 2Be reduced to weightless 1.8 * 10 -3G/cm 2
The present invention compares prior art and has following You point:
1, the inventive method is simple, prescription rationally, the defectives such as optical glass elements face burn into cut, fluffing both can have been avoided, You can improve the speed of ion-exchange, improve surface quality and the intensity of optical glass device, and be easy to promote industrial mass manufacture, its finished product rate can reach more than 95%.
2, the inventive method is applied widely, and the Yuan material of greatly having expanded Zao high strength optics glass elements product processed utilizes scope, and it is strong to carry out to the optical glass device that contains the alkali silicate glass system surperficial Zeng.
3, utilize the optical glass device product of the inventive method manufacturing, its center thickness can be less than 1 millimeter, and resistance to impact shock has improved 11 times, and bending strength improves understands 4 times, and surface hardness has improved 80%.
4, optical characteristics such as the surface smoothness of optical glass device, surface working precision and transmitance, color and luster remain intact.
5, the chemical stability of optical glass device is significantly improved, and wherein water tolerance has improved 10 times.
6, optical glass device can be with normal conventional technology edging, cutting, process, be easy to commodity production.

Claims (6)

1, a kind of surface strengthening method for optical glass elements, it has comprised the ion-exchange surface enhancement method, it is characterized in that containing the optical glass device of alkali silicate glass system, in mixed chemical solution, carry out earlier surface chemistry pre-treatment in early stage, through clean, dry, put into the mixing solutions salt bath after with its preheating and carry out ion-exchange thermal treatment, again after Xu Leng, cleaning, drying high strength optics glass elements.
2, the method for claim 1 is characterized in that the pretreated mixing solutions of surface chemistry in early stage is the aqueous solution that contains sulfuric acid and salt, and its pH value is 2~6.
3, the method for claim 1 is characterized in that the component that ion-exchange mixing dissolved salt is bathed is: KNO 390~98WT%, H 2SlO 30.5~5WT%, KOH 0~1.5WT%, KAl(SO 4) 20.8~2WT%, K 2CO 30.4~1.5WT%, Z rO 20.3~2WT%.
4,, it is characterized in that early stage, the surface chemistry pretreatment time was 0.5~5 hour (under the normal temperature) as claim 1,2 described methods.
5, as claim 1,3 described methods, it is characterized in that the ion-exchange thermal treatment temp is the softening temperature less than glass, be 350 ℃~500 ℃, heat treatment time is 5~20 hours.
6, the high-strength products that adopts surface strengthening method for optical glass elements to make, the surface that it is characterized in that containing the optical glass device of alkali silicate glass system strengthens product, especially has radius-of-curvature, optical glass device product that center thickness is little.
CN 90105773 1990-02-27 1990-02-27 Surface strengthening method for optical glass elements and high-strength products thereof Pending CN1044448A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 90105773 CN1044448A (en) 1990-02-27 1990-02-27 Surface strengthening method for optical glass elements and high-strength products thereof

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Application Number Priority Date Filing Date Title
CN 90105773 CN1044448A (en) 1990-02-27 1990-02-27 Surface strengthening method for optical glass elements and high-strength products thereof

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CN1044448A true CN1044448A (en) 1990-08-08

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003106364A1 (en) * 2002-06-13 2003-12-24 International Business Machines Corporation Ph adjustment of a melt for use in microetching glass substrates
CN100465119C (en) * 2003-05-28 2009-03-04 中央硝子株式会社 Chemically reinforced glass and method for production thereof
CN101921054A (en) * 2010-09-09 2010-12-22 浙江大学 Molten salt for chemical strengthening of glass and application process thereof
WO2011085190A1 (en) * 2010-01-07 2011-07-14 Corning Incorporated Impact-damage-resistant glass sheet
CN102690050A (en) * 2012-06-08 2012-09-26 常熟晶玻光学科技有限公司 Processing method of chemically toughened glass
CN103781739A (en) * 2011-09-09 2014-05-07 Hoya株式会社 Process for producing cover glass for potable appliance
US8978414B2 (en) 2011-11-10 2015-03-17 Corning Incorporated Acid strengthening of glass
CN107298534A (en) * 2017-05-16 2017-10-27 蚌埠市宏大制药机械有限公司 A kind of preparation method of centrifuge visor safety glass
CN107434361A (en) * 2013-07-19 2017-12-05 旭硝子株式会社 The manufacture method of chemically reinforced glass
CN113200686A (en) * 2021-05-10 2021-08-03 南通瑞景光电科技有限公司 High temperature heat treatment method for optical element

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6911261B2 (en) 2002-06-13 2005-06-28 International Business Machines Corporation pH adjustment of a melt for use in microetching glass substrates
WO2003106364A1 (en) * 2002-06-13 2003-12-24 International Business Machines Corporation Ph adjustment of a melt for use in microetching glass substrates
CN100465119C (en) * 2003-05-28 2009-03-04 中央硝子株式会社 Chemically reinforced glass and method for production thereof
US8889254B2 (en) 2010-01-07 2014-11-18 Corning Incorporated Impact-damage-resistant glass sheet
WO2011085190A1 (en) * 2010-01-07 2011-07-14 Corning Incorporated Impact-damage-resistant glass sheet
EP3670461A3 (en) * 2010-01-07 2020-08-12 Corning Incorporated Impact-damage-resistant glass sheet
CN101921054A (en) * 2010-09-09 2010-12-22 浙江大学 Molten salt for chemical strengthening of glass and application process thereof
CN103781739A (en) * 2011-09-09 2014-05-07 Hoya株式会社 Process for producing cover glass for potable appliance
US8978414B2 (en) 2011-11-10 2015-03-17 Corning Incorporated Acid strengthening of glass
US9505653B2 (en) 2011-11-10 2016-11-29 Corning Incorporated Acid strengthening of glass
CN102690050B (en) * 2012-06-08 2014-09-10 常熟晶玻光学科技有限公司 Processing method of chemically toughened glass
CN102690050A (en) * 2012-06-08 2012-09-26 常熟晶玻光学科技有限公司 Processing method of chemically toughened glass
CN107434361A (en) * 2013-07-19 2017-12-05 旭硝子株式会社 The manufacture method of chemically reinforced glass
CN107298534A (en) * 2017-05-16 2017-10-27 蚌埠市宏大制药机械有限公司 A kind of preparation method of centrifuge visor safety glass
CN113200686A (en) * 2021-05-10 2021-08-03 南通瑞景光电科技有限公司 High temperature heat treatment method for optical element

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