WO2013049988A1 - Verre optique et procédé de fabrication associé, et élément optique - Google Patents

Verre optique et procédé de fabrication associé, et élément optique Download PDF

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Publication number
WO2013049988A1
WO2013049988A1 PCT/CN2012/081538 CN2012081538W WO2013049988A1 WO 2013049988 A1 WO2013049988 A1 WO 2013049988A1 CN 2012081538 W CN2012081538 W CN 2012081538W WO 2013049988 A1 WO2013049988 A1 WO 2013049988A1
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Prior art keywords
glass
optical glass
optical
weight
less
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PCT/CN2012/081538
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English (en)
Chinese (zh)
Inventor
匡波
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成都光明光电股份有限公司
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Publication of WO2013049988A1 publication Critical patent/WO2013049988A1/fr

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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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths

Definitions

  • the invention belongs to the technical field of glass, and in particular relates to an optical glass, a manufacturing method thereof and an optical element.
  • optical systems have been increasingly developed to be high-precision, lightweight, and miniaturized, and glass having a high refractive index is suitable for use as optical components for producing small lenses;
  • the imaging quality of the optical system is closely related to the transmittance of the optical glass. The higher the transmittance of the glass, the better the imaging quality of the optical system.
  • the prior art In order to achieve the purpose of improving the optical constant consistency of the optical glass, the prior art generally performs the melting of the optical glass by a two-step melting method, that is, first, the glass batch is melted into a glass crucible, that is, clinker, and then The clinker, which knows the optical constant, is prepared in proportion and then subjected to a second fine smelting to obtain a high quality optical glass blank.
  • a glass crucible that is, clinker
  • the clinker which knows the optical constant
  • platinum or quartz crucible is generally used, and platinum is used to increase the use and consumption of expensive platinum, increase the manufacturing cost of glass, and in the process of clinker smelting, platinum.
  • the optical glass needs to meet the following requirements, that is, the etching of the quartz crucible by the molten glass at the required melting temperature. The amount should be as low as possible.
  • the large amount of wear of the quartz crucible will not only increase the preparation cost of the glass, but also change the composition of the glass, affecting the refractive index and transmittance of the optical glass. Optical performance.
  • the optical glass when the optical glass is formed into a glass material such as a strip, a block or a bar, if the viscosity of the molten glass is too small at the molding temperature, the glass liquid may be streaked due to internal convection or the like, and usually such stripes are Known as forming strips, forming strips reduce the optical properties of the glass, which reduces the imaging quality of the optical system.
  • the technical problem to be solved by the present invention is to provide an optical glass, a manufacturing method thereof, and an optical element.
  • the optical glass provided by the present invention has a refractive index of 1.99 or more, an Abbe number of 23 or more, and a glass forming viscosity of 4.5 poise. The above, not only the optical performance is good, but also the molding performance is good.
  • the invention provides an optical glass, comprising:
  • Gd 2 0 3 0 ⁇ 15 ⁇ % of Gd 2 0 3 , Y 2 0 3 and Yb 2 0 3 , wherein Gd 2 0 3 is 0 to 12 wt%;
  • 31 wt% to 45 wt% of La 2 O 3 is included .
  • it comprises 32.5 wt% to 38 wt% of La 2 O 3 .
  • it comprises 0.5wt ⁇ 15wt°/c ⁇ Gd 2 0 3 , Y 2 0 3 and Yb 2 0 3 , wherein Gd 2 0 3 is 0.5 wt% to 8 wt%.
  • 13 wt% to 22 wt% of Ti0 2 is included .
  • it comprises 8.2 wt% to 14 wt% of Nb 2 0 5 .
  • more than 5 wt% and less than 15 wt% of BaO are included.
  • more than 10% by weight and less than 15% by weight of BaO are included.
  • it comprises 3 wt% to 9 wt% of Zr0 2 .
  • more than 5.5 wt% and less than 8 wt% of B 2 O 3 are included .
  • the optical glass has the following properties:
  • the refractive index is 1.99 or more
  • the Abbe number is 23 or more
  • the viscosity of the glass liquid phase is 4.5 poise or more
  • the corresponding wavelength ⁇ 7 () is 455 nm or less.
  • the invention also provides a method for manufacturing optical glass, comprising the following steps:
  • the optical glass clinker is subjected to secondary fine melting, clarified, and homogenized to obtain an optical glass.
  • the present invention also provides an optical element formed of the optical glass described in the above technical solution. Compared with the prior art, the optical glass provided by the present invention comprises: 5 wt% to 10 wt. /c ⁇ Si0 2 ; 10wt% ⁇ 18wt.
  • the present invention introduces 5 wt% to 10 wt% of SiO 2 in the optical glass, which not only effectively increases the viscosity of the glass liquid phase, but also reduces the glass liquid.
  • the amount of etching of quartz crucible is more significantly reduced; the invention introduces more than 30 wt% and less than or equal to 50 wt% in the optical glass.
  • the invention introduces 10 wt% to 22 wt ° / ⁇ Ti 0 2 in the optical glass, which significantly increases the refraction of the glass Rate, effectively reducing the density of the glass, while introducing more than 2wt% To 15wt% of BaO, Ti0 2 is introduced to effectively improve the degree of coloring caused by such phenomena deteriorates.
  • the present invention by optimizing the glass formulation, to obtain an optical glass having good optical properties not only a higher refractive index, Abbe number, etc. And having a high glass liquid viscosity and other good molding properties.
  • the optical glass provided by the present invention has a refractive index of 1.99 or more; Abbe number is 23 or more; glass liquid viscosity reaches 4.5 poise or more; transmittance When the ratio reaches 70%, the corresponding wavelength ⁇ 7 () is 455 nm or less.
  • the invention provides an optical glass, comprising:
  • Gd 2 0 3 0 ⁇ 15 ⁇ % of Gd 2 0 3 , Y 2 0 3 and Yb 2 0 3 , wherein Gd 2 0 3 is 0 to 12 wt%;
  • Si0 2 is an important form of forming an optical oxide.
  • the optical constant of the glass is adjusted, but also the anti-devitrification effect of the glass is maintained, and by adjusting the content thereof, the viscosity of the glass liquid phase is effectively increased, and the viscosity is lowered.
  • the content of Si0 2 when the content of Si0 2 is less than 5% by weight, the effect of increasing the viscosity of the liquid phase of the glass cannot be achieved; when the content is more than 10% by weight, the melting property of the glass is deteriorated, and it is difficult to achieve a high refractive index; therefore, the content of Si0 2 It is limited to 5 wt% to 10 wt%, preferably 6 wt% to 9 wt%, more preferably 6.5 wt% to 8.5 wt%.
  • B 2 0 3 is also a bulk oxide of glass, which can effectively improve the thermal stability and chemical stability of the glass, increase the resistance to devitrification of the glass, increase the dissolution rate of the glass to the high refractive index oxide, and increase the glass.
  • the total content of B 2 O 3 and SiO 2 is from 10% by weight to 18% by weight, preferably from 12% by weight to 18% by weight, more preferably from 12.5% by weight to 16% by weight.
  • the inventors have found through research that when the content of Si0 2 is kept higher than or equal to the content of B 2 0 3 , the vitreous quartz crucible can be significantly lowered.
  • Etching amount of the crucible Further, if the content of Si0 2 content greater than or equal to 0 3 B 2, especially 0 3 content is controlled within a range of more than 8wt% and less than 5.5wt%, and preferably from 6wt% ⁇ 7.5wt%
  • the optical glass can not only maintain a high refractive index but also have a high glass liquid viscosity, can produce a glass blank without forming streaks, and can solve the problem that the Si0 2 content is greater than or equal to the B 2 0 3 content.
  • the problem of deterioration of glass coloration and the like makes the optical glass of the obtained optical fiber have better light transmission performance.
  • La 2 0 3 is an essential component for obtaining a high refractive index glass, and the present invention ensures the optical constant of the optical glass by introducing an appropriate amount of La 2 O 3 while reducing the B 2 0 3 content; when La 2 0 3 When the content is 30% by weight or less, the refractive index of the glass is insufficient; when the content is more than 50% by weight, the devitrification resistance of the glass is lowered, and it is difficult to obtain a glass which can be stably produced. Therefore, the present invention will La 2 0 3 The content is limited to more than 30% by weight and less than or equal to 50% by weight, preferably from 31% by weight to 45% by weight, more preferably from 32.5% by weight to 38% by weight.
  • Yb 2 0 3 , Y 2 0 3 and Gd 2 0 3 all have the effect of increasing the refractive index of the glass and reducing the dispersion.
  • the total content of Yb 2 0 3 , Y 2 0 3 and Gd 2 0 3 is 0 ⁇ 15 wt%, preferably 0.5 wt% to 15 wt%, more preferably 1 wt% to 14 wt%.
  • Gd 2 0 3 can not only increase the refractive index of the glass, but also reduce the dispersion of the glass, and can be mixed with a high refractive index oxide such as La 2 0 3 to improve the production stability of the glass.
  • the content of the Gd 2 0 3 is 0 wt% to 12 wt%, preferably 0.5 wt% to 8 wt%, more preferably 0.5 wt% to 2.5 wt%.
  • the content of the Gd 2 0 3 content is less than 0.5% by weight, although the refractive index and the dispersion are lowered, the effect is not remarkable; when the Gd 2 0 3 content is more than 12% by weight, the glass resistance is lowered.
  • the content of the Yb 2 0 3 is preferably 0 wt% to 2 wt%, more preferably 0.1 wt% to 0.8 wt%; and the content of Y 2 0 3 is preferably 0 wt% to 2 wt%, more preferably 0.1. Wt% ⁇ lwt%.
  • Nb 2 0 5 can increase the refractive index of the glass and can improve the resistance to devitrification of the glass.
  • the content is 8 wt% or less, the above effect is not obvious, but when the content of Nb 2 0 5 is 15 wt% or more, the transmission of the glass The rate deteriorates, especially the transmittance on the short-wavelength side sharply deteriorates; therefore, the present invention limits the content of Nb 2 0 5 to more than 8 wt% to less than 15 wt%, preferably from 8.2 wt% to 14 wt%, more preferably 8.2 wt%. 12wt%.
  • Ti0 2 can significantly increase the refractive index of the glass and enhance the chemical stability, and an appropriate amount of introduction can also effectively reduce the glass density, but when the Ti0 2 content is less than 10 wt%, the low-density performance of the glass is not obvious, and the content thereof exceeds 22wt%, glass transition temperature rises sharply, glass The coloring is increased. Therefore, the present invention limits the content of Ti0 2 to 10 wt% to 22 wt%, preferably 13 wt% to 22 wt%, more preferably 19.2 wt% to 22 wt%, and most preferably 19.5 wt% to 21.8 wt%. It is also preferably from 19.7 wt% to 21.5 wt%.
  • BaO can effectively adjust the optical constant of the glass.
  • the dispersion can be reduced, but also the phenomenon of poor coloration due to the introduction of Ti0 2 can be effectively improved, and the chemical stability can be improved.
  • the carbonate or nitrate form also has the effect of promoting glass defoaming when used as a raw material; in the present invention, the BaO content is more than 2% by weight and less than 15% by weight, preferably more than 5% by weight and less than 15% by weight, more preferably More than 10 wt% is less than 15 wt%, and most preferably 12 wt% to 14 wt%.
  • the content of BaO is 2% by weight or less, the effect is not remarkable, and when the content is 15% by weight or more, the glass resistance is impaired, and it is difficult to obtain a glass which can be stably produced.
  • Wo 3 can increase the refractive index of the optical glass, and when it is added in a small amount, the devitrification resistance of the glass can also be improved.
  • an appropriate amount of introduction can also effectively improve the crystallization property of the glass.
  • the present invention limits the content of W0 3 to 0 wt% to 6 wt%, preferably 0.1 wt% to 3 wt%, more preferably 0.4 wt% to 1 wt%.
  • ZnO can lower the glass transition temperature of glass, and can also improve the anti-devitrification of glass and reduce the viscous flow temperature of glass.
  • the content of ZnO is from 0.5 wt% to 5 wt%, preferably from 1.5 wt% to 4 wt%, more preferably from 1.5 wt% to 2.5 wt%.
  • the ZnO content is less than 0.5% by weight, the glass transition temperature of the glass is not significantly lowered; when the content of ZnO is more than 5% by weight, the refractive index of the glass is lowered.
  • Zr0 2 can moderately increase the refractive index and thermal stability of the glass, and when it is added in a small amount, it can improve the devitrification resistance of the glass. However, if the amount of addition is too large, the devitrification resistance of the glass is drastically lowered.
  • the invention limits the content of ZrO 2 to 2 wt% to 10 wt%, preferably 3 wt% to 9 wt%, more preferably 5 wt% to 7 wt%.
  • CaO, SrO, and MgO may be appropriately introduced in the present invention, and the total content of CaO, SrO, and MgO is from 0 wt% to 10 wt%, preferably from 0 wt% to 5 wt%, more preferably from 0.5 wt% to 3.5 wt%; wherein, CaO
  • the content of MgO is preferably 0 wt% to 1 wt%, more preferably 0.5 wt% to 1 wt%;
  • the content of SrO is preferably 0 wt% to 8 wt%, more preferably 0.1 wt% to 5 wt%; and the content of MgO is preferably 0 wt% to 2 wt%.
  • Sb 2 0 3 and Sn0 2 can be used not only for defoaming but also for the melting atmosphere of the glass.
  • the present invention limits the content of Sb 2 0 3 to 0 wt% to 0.1 wt%, preferably 0.005 wt% to 0.09 wt%, more preferably 0.01 wt% to 0.08 wt%; and the content of Sn0 2 is limited to 0 wt% to 0.9 wt. % is preferably 0.001% by weight to 0.85% by weight, more preferably 0.01% by weight to 0.08% by weight.
  • the obtained optical glass not only has good optical properties such as high refractive index and Abbe number, but also has good molding properties such as high glass liquid viscosity.
  • the refractive index of the optical glass is preferably 1.99 or more, more preferably 1.993 or more, most preferably 1.995 or more, and most preferably 2.0 to 2.1; and the Abbe number is preferably 23 or more, and more preferably 24 or more.
  • the glass liquid viscosity is preferably 4.5 poise or more, more preferably 4.7 poise or more, most preferably 5 poise or more, and most preferably 5.5 poise or more;
  • the wavelength ⁇ 7 () corresponding to 70% is preferably 455 nm or less, more preferably 454 nm or less, and most preferably 450 nm or less.
  • the invention also provides a method for manufacturing optical glass, comprising the following steps:
  • optical glass clinker is subjected to secondary fine melting, clarified, homogenized, and cooled to obtain an optical glass.
  • the oxide, hydroxide, carbonate or nitrate of the component described in the above technical solution is used as a raw material, and the mixture is thoroughly mixed and placed in a quartz crucible for the first smelting. Since the silica content in the glass is high, the etching of the quartz crucible is small, so that the cost can be reduced.
  • the temperature of the first smelting is preferably from 1160 °C to 1200 °C, more preferably from 1170 °C to 1190 °C.
  • a glass clinker which is commonly known as a glass crucible
  • the glass clinker is subjected to secondary refining, and after the glass is clarified and homogenized, a molten glass is obtained.
  • the secondary finish smelting is preferably carried out in a platinum crucible, and the temperature of the finish smelting is preferably from 1280 °C to 1350 °C, more preferably from 1290 °C to 1340 °C.
  • the finely smelted glass liquid is lowered into a preheated metal mold by dropping to 1,250 ° C, preferably 1200 ° C or less, according to a method well known to those skilled in the art, and quenching to obtain an optical glass.
  • the performance test of the optical glass is as follows:
  • the refractive index (nd) value is (-2 ° C / h) - ( -6 ° C / h) annealing value, refractive index and Abbe number according to the colorless optics provided in GB/T 7962.1-1987 Measurement of refractive index and dispersion coefficient of glass Test method to test;
  • the glass was made into a sample having a thickness of 10 mm ⁇ 0.1 mm, and the glass was tested to have a transmittance of 70% corresponding to the wavelength ⁇ 7 () .
  • the viscosity is tested using a BROOKFIELD DV- ⁇ ULTRA type high temperature rotational viscometer or a plate viscometer.
  • a glass crucible of about 50 cm 3 was placed in a plurality of platinum crucibles, and then placed in a ladder furnace with a temperature gradient of 10 ° C for two hours. The glass was taken out and cooled, and the glass was not observed. The lowest temperature of crystallization is the liquidus temperature.
  • optical glass provided by the present invention has been tested to have the following properties:
  • the refractive index is 1.99 or more
  • the Abbe number is 23 or more
  • the liquidus viscosity is above 4.5 poise
  • the corresponding wavelength ⁇ 7 () is 455 nm or less.
  • the present invention also provides an optical element formed by the optical glass described in the above technical solution in accordance with a method well known to those skilled in the art. Since the optical glass has a high refractive index and a high transmittance, the optical element also has a high refractive index and a high transmittance, and can be applied to devices such as digital cameras, digital video cameras, and camera phones.
  • the optical glass provided by the present invention comprises: 5 wt% to 10 wt. /c ⁇ Si0 2 ; 10wt% ⁇ 18wt. / ( ⁇ B 2 0 3 and Si0 2, wherein, Si0 2 ⁇ B 2 0 3; greater than 30wt% and 50wt% or less of La 2 0 3; 0 ⁇ 15 ⁇ % of Gd 2 0 3, Y 2 0 3 And Yb 2 0 3 , wherein Gd 2 0 3 is 0 to 12 wt%; 10 wt% to 22 wt% of Ti0 2 ; more than 8 wt% and less than 15 wt% of Nb 2 0 5 ; 0.5 wt% to 5 wt% of ZnO; ⁇ 6wt% of W0 3 ; 2wt% ⁇ 10wt° / ⁇ Zr0 2 ; more than 2wt% and less than 15wt% of BaO; 0 ⁇ 10wt%
  • Example 1 ⁇ 14 Glass composition w According to the following steps, optical glass is produced according to the ratio of raw materials shown in Table 1 and Table 2:
  • the molten glass is lowered to 1200 ° C or lower, poured into a preheated metal mold, and cooled to obtain an optical glass.
  • the optical glass was subjected to performance test, and the results are shown in Table, Table 1 and Table 2 are performance parameters of the optical glass prepared in the examples of the present invention.
  • the optical glass was prepared according to the ratio of raw materials shown in Table 1 and Table 2:
  • the raw materials described in Table 1 were thoroughly mixed and placed in a quartz crucible. After the first melting, the glass crucible was formed, and then the glass crucible was formed. Put into the platinum crucible, the second fine smelting, after the glass is clarified and homogenized, the molten glass is obtained;
  • the molten glass is lowered to 1200 ° C or lower, poured into a preheated metal mold, and cooled to obtain an optical glass.
  • the optical glass was subjected to performance test, and the results are shown in Table, Table 1 and Table 2 are performance parameters of the optical glass prepared in the examples of the present invention.
  • the optical glass provided by the present invention has a high refractive index and a high transmission.

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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)
  • Glass Compositions (AREA)

Abstract

La présente invention concerne un verre optique qui comprend 5 % en poids-10 % en poids de SiO2 ; 10 % en poids-18 % en poids d'un mélange de B2O3 et SiO2, avec SiO2≥B2O3 ; plus de 30 % en poids et 50 % en poids ou moins de La2O3 ; 0-15 % en poids d'un mélange de Gd2O3, Y2O3 et Yb2O3, la teneur en Gd2O3 étant de 0-12 % en poids ; 10 % en poids-22 % en poids de TiO2 ; plus de 8 % en poids et moins de 15 % en poids de Nb2O5 ; 0,5 % en poids-5 % en poids de ZnO ; 0-6 % en poids de WO3 ; 2 % en poids-10 % en poids de ZrO2 ; plus de 2 % en poids et moins de 15 % en poids de BaO ; 0-10 % en poids d'un mélange de CaO, SrO et MgO, la teneur en SrO étant de 0-8 % en poids ; 0-0,1 % en poids de Sb2O3 ; et 0-0,9 % en poids de SnO.
PCT/CN2012/081538 2011-10-08 2012-09-18 Verre optique et procédé de fabrication associé, et élément optique WO2013049988A1 (fr)

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CN201110301859.2 2011-10-08
CN 201110301859 CN102503120B (zh) 2011-10-08 2011-10-08 光学玻璃及其制造方法、光学元件

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110590155A (zh) * 2019-10-11 2019-12-20 成都光明光电股份有限公司 光学玻璃、玻璃预制件、光学元件及光学仪器
WO2022055709A1 (fr) * 2020-09-10 2022-03-17 Corning Incorporated Verres à base de silicoborate et de borosilicate ayant un indice de réfraction élevé et une transmittance élevée à la lumière bleue
US11802073B2 (en) 2020-09-10 2023-10-31 Corning Incorporated Silicoborate and borosilicate glasses with high refractive index and low density
US11999651B2 (en) 2020-09-10 2024-06-04 Corning Incorporated Silicoborate and borosilicate glasses having high refractive index and low density

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CN102503120B (zh) * 2011-10-08 2013-02-20 成都光明光电股份有限公司 光学玻璃及其制造方法、光学元件
CN104788018B (zh) * 2014-01-22 2019-03-05 成都光明光电股份有限公司 高折射高色散光学玻璃、光学元件及光学仪器
CN105837029B (zh) * 2016-04-25 2019-06-07 湖北新华光信息材料有限公司 光学玻璃、其制备方法及光学元件
CN110510869B (zh) * 2018-05-22 2021-06-22 成都光明光电有限责任公司 光学玻璃
CN109694199A (zh) * 2019-02-13 2019-04-30 安徽金冠玻璃有限责任公司 一种高透明度玻璃瓶的生产工艺
DE102022125160A1 (de) 2022-09-29 2024-04-04 Schott Ag Hochbrechendes Glas

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JPS5950048A (ja) * 1982-09-16 1984-03-22 Ohara Inc 光学ガラス
US4584279A (en) * 1983-12-01 1986-04-22 Schott Glaswerke Optical glass with refractive indices>1.90, Abbe numbers>25 and high chemical stability
JP2010215503A (ja) * 2002-12-27 2010-09-30 Hoya Corp 光学ガラス、プレス成形用ガラスゴブおよび光学素子
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110590155A (zh) * 2019-10-11 2019-12-20 成都光明光电股份有限公司 光学玻璃、玻璃预制件、光学元件及光学仪器
CN110590155B (zh) * 2019-10-11 2022-04-15 成都光明光电股份有限公司 光学玻璃、玻璃预制件、光学元件及光学仪器
WO2022055709A1 (fr) * 2020-09-10 2022-03-17 Corning Incorporated Verres à base de silicoborate et de borosilicate ayant un indice de réfraction élevé et une transmittance élevée à la lumière bleue
US11802073B2 (en) 2020-09-10 2023-10-31 Corning Incorporated Silicoborate and borosilicate glasses with high refractive index and low density
US11976004B2 (en) 2020-09-10 2024-05-07 Corning Incorporated Silicoborate and borosilicate glasses having high refractive index and high transmittance to blue light
US11999651B2 (en) 2020-09-10 2024-06-04 Corning Incorporated Silicoborate and borosilicate glasses having high refractive index and low density

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TWI466841B (fr) 2015-01-01
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CN102503120B (zh) 2013-02-20

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