WO2008046300A1 - High-refractivity low-dispersion optical glass for precise press molding - Google Patents

High-refractivity low-dispersion optical glass for precise press molding Download PDF

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Publication number
WO2008046300A1
WO2008046300A1 PCT/CN2007/002921 CN2007002921W WO2008046300A1 WO 2008046300 A1 WO2008046300 A1 WO 2008046300A1 CN 2007002921 W CN2007002921 W CN 2007002921W WO 2008046300 A1 WO2008046300 A1 WO 2008046300A1
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Prior art keywords
glass
content
optical
press molding
refractive index
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PCT/CN2007/002921
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French (fr)
Chinese (zh)
Inventor
Bo Kuang
Wei Sun
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Cdgm Glass Co., Ltd
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Application filed by Cdgm Glass Co., Ltd filed Critical Cdgm Glass Co., Ltd
Priority to KR1020087025530A priority Critical patent/KR101048238B1/en
Priority to JP2009510265A priority patent/JP5094846B2/en
Publication of WO2008046300A1 publication Critical patent/WO2008046300A1/en

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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 present invention relates to an optical glass, and more particularly to a high refractive index low dispersion optical glass having a refractive index (Nd) of 1.77 to 1.84 and an Abbe number (Vd) of 36 to 44.
  • the so-called precision molding is to mold a glass preform with a high-precision mold having a predetermined product shape under a certain temperature and pressure, thereby obtaining a glass product having a final product shape (or very close to the final product shape) and having an optical functional surface.
  • Aspherical lenses made by precision molding technology usually do not need to be polished and polished to achieve high productivity and low cost.
  • Various optical glass components such as spherical lenses, aspherical lenses, prisms, diffraction gratings, etc. can now be manufactured by precision molding techniques.
  • transition temperature (Tg) and softening temperature (Ts) of the glass material are required to be as low as possible.
  • Confirmation Optical glass for aspherical lenses, glass with various optical constants, optical glass with Nd of 1.77- 1.84, Vd of 36-44 is used in modern advanced imaging equipment, including lead and antimony. Such optical glass is not produced and used because it is harmful to the environment.
  • the optical glass containing no lead or antimony is usually B 2 0 3 (Si0 2 ) — La 2 0 3 — Nb 2 0 5 (Ta 2 0 5 )
  • a RO (R stands for alkaline earth metal) system the softening temperature of glass is usually much higher than 600 ° C, not suitable for precision molding.
  • U.S. Patent No. 2,003,032, 542 discloses an optical glass of a B 2 0 3 (Si0 2 ) — La 2 0 3 — Gd 2 0 3 — Nb 2 0 5 — Zr0 2 system having a refractive index of 1.80 or more, Abbe The number is around 40, but the glass transition temperature is above 650 ° C, which is not suitable for precision molding materials.
  • Japanese Patent Publication No. 06-305769 discloses an optical glass for precision molding of a Si0 2 - B 2 0 3 - La 2 0 3 - Ta 2 0 5 - ZnO- Li 2 0 system, which is also used in a large amount of glass.
  • Japanese Patent Laid-Open No. 2002-362938 discloses a B 2 0 3 -Si0 2 -La 2 0 3 - ZnO ⁇ Nb 2 0 5 - Ta 2 0 5 - W0 3 system and a B 2 0 3 disclosed in Japanese Laid-Open Patent Publication No. 2002-012443 - Si0 2 - La 2 0 3 - Li 2 0- ZnO- Nb 2 0 5 - Ta 2 0 5 - W0 3 system, although a lower softening temperature can be achieved, a certain amount of Ta 2 0 5 is used , Glass is expensive.
  • the technical problem to be solved by the present invention is to provide an optical glass for high refractive index and low dispersion precision molding, which is free from environmentally harmful substances such as lead, arsenic and cadmium, and does not contain expensive Ta 2 0 5 , glass.
  • the softening temperature meets the requirements for precision molding.
  • the optical glass for high refractive index and low dispersion precision molding has a weight percentage composition of: Si0 2 : 1-8%, B 2 0 3 : 16-30%, La 2 0 3 : 15—40%, Gd 2 0 3 : 0—20%, ZnO: 8—30%, Nb 2 0 5 : 0. 5—14. 5%, W0 3 : 0—12.
  • the beneficial effects of the present invention are as follows:
  • the present invention adopts a B 2 0 3 _Si0 2 — La 2 0 3 (Gd 2 0 3 )-ZnO system, and uses a reasonable ratio of Nb 2 0 5 , W0 3 , Ti0 2 to achieve the desired glass.
  • the optical glass transition temperature (Tg) of the present invention is lower than 560 ° C, and the composition does not contain high-priced Ta 2 0 5 , and the glass has good chemical stability and can be used in equipment such as single crucible or continuous melting furnace. Stable production in batches, suitable for low-cost precision molding of optical components such as aspherical lenses.
  • B 2 0 3 is a glass network-forming body oxide and is an essential component of a glass network. Especially in a high refractive index lanthanum glass, B 2 0 3 is a main component for obtaining a stable glass. When the content of B 2 0 3 is less than 16%, the melting property of the glass is deteriorated, and the devitrification resistance is not satisfactory; when the content of 0 3 is higher than 30%, the refractive index of the glass does not reach the design goal, so B 2 0 3
  • the preferred content (weight percent content, hereinafter the same) is from 16% to 30%, more preferably from 19% to 26%.
  • the 510 2 is also a network-forming body oxide for forming glass.
  • Si0 2 By adding a certain amount of Si0 2 , the high-temperature viscosity of the glass can be increased, and the devitrification resistance and chemical stability of the glass can be improved.
  • the content is less than 1%, the production process performance of the glass is poor, that is, the aforementioned effect is not obvious.
  • the refractive index of the glass exceeds 8%, the devitrification resistance is deteriorated, and at the same time, the raw material is difficult to be melted during production, so the SiO 2 content is preferably 1 to 8%, more preferably 1 to 6%.
  • La 2 0 3 is a main component of the high-refraction low-dispersion lanthanide optical glass, and is used for increasing the refractive index of the glass without significantly increasing the dispersion of the glass.
  • the glass resistance can be improved.
  • Devitrification properties improve the chemical stability of the glass.
  • the content of La 2 O 3 is less than 15%, the above effects are not obtained, and when the content exceeds 40%, the devitrification property of the glass is deteriorated, so the La 2 O 3 content is preferably 15 to 40%.
  • Gd 2 0 3 is similar to that of La 2 0 3 , which also increases the refractive index of the glass and does not significantly increase the dispersion of the glass, and has the effect of improving the chemical stability and devitrification resistance of the glass in physical and chemical properties.
  • the devitrification resistance of the glass can be appropriately increased, but the specific gravity of the glass can be increased.
  • the content of Gd 2 0 3 is preferably from 0 to 20%, more preferably from 5 to 15%.
  • La 2 0 3 and Gd 7 (the total content of ⁇ is not less than 20%, but when the total content of LaA and Gd, 0; %, glass The stability is deteriorated, the devitrification resistance is lowered, and the softening temperature is sharply increased, so the total content of La 2 O 3 and Gd 2 0 3 is preferably 20 to 45%.
  • ZnO is an essential component of the glass of the present invention, which is advantageous for lowering the melting temperature and softening temperature of the glass, and for adjusting the optical properties of the glass.
  • the content is less than 8%, the softening temperature of the glass increases; and when the content is more than 30%, the dispersion of the glass increases, the crystallization tendency increases, and the high temperature viscosity of the glass becomes small, which brings about a great glass forming. It is difficult, so the content of ZnO is preferably from 8 to 30%, more preferably from 12 to 28%.
  • Nb 2 0 5 is an effective component for increasing the refractive index of the glass.
  • the content is less than 0.5%, the refractive index of the glass does not reach the design goal, and when the content is higher than 14.5%, the glass softens. 5 ⁇ 14. 5% ⁇
  • the content of the Nb 2 0 5 is preferably 0. 5-14. 5%.
  • W0 3 has the effect of increasing the refractive index and dispersion of the glass and improving the crystallization property of the glass.
  • the experiment shows that when the content exceeds 12.5%, the devitrification resistance of the glass is decreased, so the preferred content of W0 3 is 0-12. 5%, more preferably 0-8%.
  • Ti0 2 is effective for increasing the refractive index and dispersion of the glass, and can improve the water resistance of the glass and lower the specific gravity of the glass.
  • Ti0 2 also functions to increase the high temperature viscosity of the glass to improve the crystallization property of the glass.
  • the Ti0 2 content is preferably from 0 to 9%. 5 ⁇ 24 ⁇
  • the sum of the content of the above Nb 2 0 5 , W0 3 and Ti0 2 is 6.5 - 24%.
  • Li 2 0 is the most effective component for lowering the transition temperature and softening temperature of the glass, and Li 2 0 has a stronger fluxing effect. 5 - 4
  • the preferred content of Li 2 0 is 0. 5 — 4
  • the preferred content of Li 2 0 is 0. 5— 4 5 ⁇ 3% ⁇ The %, more preferably 0. 5 - 3%.
  • ⁇ 2 has an effect of improving the resistance to devitrification of the glass and improving the chemical stability, and also serves to increase the refractive index and reduce the dispersion in the bismuth-based glass.
  • the content is less than 1%, the above effect is not obtained; when the content is more than 10%, the glass softening temperature is increased, and the glass resistance to devitrification is deteriorated. Therefore, the preferred content of Zr0 2 is from 1 to 10%.
  • Y 2 0 3 , Yb 2 0 3 and Lu 2 0 3 have the effects of improving glass stability and devitrification resistance, and can also adjust the optical constant of the glass, but when the content exceeds 5%, the glass transition temperature is increased. Therefore, Y 2 0 3 is preferably present in an amount of from 0 to 5%, more preferably not added; Yb 2 0 3 is preferably present in an amount of from 0 to 5%, more preferably not Addition; Lu 2 0 3 is preferably present in an amount of from 0 to 5%, more preferably not added.
  • Na 2 0 has the effect of lowering the glass transition temperature and increasing the transparency of the glass.
  • the content of ⁇ 0 is preferably 0 to 3%. More preferably, the content is 0-1%.
  • ⁇ 20 is similar to that of Na 2 0, and its preferred content is 0 to 2%, more preferably not added.
  • A1 2 0 3 can improve the chemical stability of the glass and increase the high temperature viscosity of the glass. However, when the content is higher than 2%, the devitrification resistance of the glass is lowered, and the melting difficulty is increased. Therefore, A1 2 0 3 is preferably 0 - 2%, more preferably not added.
  • the BaO can reduce the dispersion of the glass while improving the transmittance of the glass.
  • the content exceeds 3%, the refractive index target of the glass cannot be achieved, and the crystallization tendency of the glass is increased. Therefore, the BaO preferably has a content of from 0 to 3%.
  • CaO can improve the chemical stability of the glass and has a fluxing effect, but when the content is higher than 3%, the crystallization tendency of the glass increases. Therefore, CaO is preferably contained in an amount of from 0 to 3%, more preferably not added.
  • MgO and SrO are similar to that of CaO, which improves the homogeneity of the glass.
  • the MgO content is preferably from 0 to 3%, more preferably not added; and the SrO is preferably from 0 to 3%, more preferably not added.
  • Sb 2 0 3 and Sn0 2 are used as a defoaming agent, and the content of Sb 2 0 3 is preferably 0-0.5%, more preferably not added; and the content of Sn0 2 is preferably 0-0.5%, more preferably not added.
  • the present invention does not use components such as Pb0, As 2 0 3 and CdO.
  • the production method of the present invention is:
  • the oxide, hydroxide, carbonate, and nitrate raw materials corresponding to the composition are weighed in proportion, thoroughly mixed, added to a platinum crucible or a continuous melting furnace, and melted, clarified, and homogenized at 1240-132 CTC. After cooling, the molten glass liquid is poured into the preheated metal mold, and the glass is placed in the annealing furnace together with the metal mold, and is obtained by quenching and annealing.
  • Table 1 Table 2, Table 3 and Table 4 list 24 examples and 3 comparative examples of the present invention, which list the refractive index (Nd), Abbe number (Vd), and transition temperature of the glass ( Tg), density (d), and transmittance ratios of 80% and 5% (expressed by ⁇ 80 and ⁇ 5 , respectively). 9
  • the refractive index (Nd) of the optical glass of the present invention is 1.77 - 1.84
  • the Abbe number (Vd) is 35 - 43
  • the glass transition temperature does not exceed 560 ⁇
  • the chemical stability is excellent
  • the devitrification resistance is obtained.
  • a good degree of coloring the proportion of small, very suitable for precision press molding an optical element aspherical lens, a spherical lens or the like, and does not contain glass components ⁇ 0 5 expensive raw materials, low cost, has a competitive advantage.

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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)
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  • Glass Compositions (AREA)

Abstract

The invention provides a high-refractivity and low-dispersion optical glass suitable for precise press molding, and the glass comprises, in wt%, SiO2 1-8, B2O3 16-30, La2O3 15-40, Gd2O3 0-20, ZnO 8-30, Nb2O5 0.5-14.5, WO3 0-12.5, TiO2 0-9, Li2O 0.5-4, ZrO2 1-10, Y2O3 0-5, Yb2O3 0-5, Lu2O3 0-5, Na2O 0-3, K2O 0-2, Al2O3 0-2, BaO 0-3, CaO 0-3, SrO 0-3, MgO 0-3, Sb2O3 0-0.5, and SnO2 0-0.5. The invention adopts a B2O3-SiO2-La2O3(Gd2O3)-ZnO glass system, and adjusts contents of Nb2O5, WO3 and TiO2 to a reasonable proportion to make glass have the required optical constants and good physicochemical properties suitable for precise press molding. The glass has a transformation temperature (Tg) of lower than 560 ºC, but does not comprise expensive Ta2O5, meanwhile it has good chemical resistance, can be stably produced in large scale with a single pot, a continuous smelting furnace, etc., and is suitable for precise press molding of asphericallenses and other optical components in a low cost.

Description

高折射率低色散精密压型用光学玻璃 所属技术领域  Optical glass for high refractive index and low dispersion precision molding
本发明涉及一种光学玻璃， 特别是涉及一种具有折射率 (Nd) 为 1. 77 一 1. 84， 阿贝数 （Vd) 为 36— 44的高折射率低色散光学玻璃。  The present invention relates to an optical glass, and more particularly to a high refractive index low dispersion optical glass having a refractive index (Nd) of 1.77 to 1.84 and an Abbe number (Vd) of 36 to 44.
背景技术 Background technique
随着光电产品市场的激烈竞争和发展， 高产率、 低成本地制造光学元 件是每一个光学材料和光学元件制造商的目标。采用精密模压成型技术 (包 括直接压型法和二次压型法)可以减少原料消耗，大大降低光学元件的机械 加工量从而降低人力物力成本， 并可以较容易实现批量稳定生产， 同时还 可以减轻环境污染。 另一方面， 近年来数码相机、 数字摄像机、 照相手机 等日益流行， 用于光学系统的机械设备的集成度及功能迅速增加。 在这种 情况下， 要求光学系统达到更高的准确度， 并减轻光学系统的重量和减小 尺寸。 目前解决这一问题的主要方法是采用非球面镜， 使用非球面元件已 成为光学设计的主流， 非球面透镜的制造则广泛使用精密模压的方法。  With the fierce competition and development of the optoelectronics market, high-yield, low-cost manufacturing of optical components is the goal of every optical material and optical component manufacturer. The use of precision molding technology (including direct compression molding and secondary compression molding) can reduce raw material consumption, greatly reduce the mechanical processing of optical components, thereby reducing the cost of manpower and material resources, and can easily achieve batch stable production, while also reducing Environmental pollution. On the other hand, in recent years, digital cameras, digital video cameras, camera phones, and the like have become increasingly popular, and the integration and functions of mechanical devices for optical systems have rapidly increased. In this case, the optical system is required to achieve higher accuracy and reduce the weight and size of the optical system. At present, the main method to solve this problem is to use an aspherical mirror. The use of aspherical components has become the mainstream of optical design, and the manufacture of aspherical lenses is widely used in precision molding.
所谓精密模压， 就是在一定的温度、 压力下， 用具有预定产品形状的 高精密模具模压玻璃预制件，从而获得具有最终产品形状 (或非常接近于最 终产品形状)并具有光学功能面的玻璃制品。采用精密模压技术制造的非球 面透镜通常不用再进行研磨抛光， 从而达到高产率低成本的目的。 现在通 过精密模压技术可以制造各种光学玻璃元件产品如球面透镜、非球面透镜、 棱镜、 衍射光栅等。  The so-called precision molding is to mold a glass preform with a high-precision mold having a predetermined product shape under a certain temperature and pressure, thereby obtaining a glass product having a final product shape (or very close to the final product shape) and having an optical functional surface. . Aspherical lenses made by precision molding technology usually do not need to be polished and polished to achieve high productivity and low cost. Various optical glass components such as spherical lenses, aspherical lenses, prisms, diffraction gratings, etc. can now be manufactured by precision molding techniques.
在进行精密模压成型时， 为了将高精密的模面复制在玻璃成型品上， 需要在高温下 （通常在玻璃软化点温度以上 15-4CTC ) 加压成型玻璃预制 体， 这时成型模被暴露在高温中且被施以较高的压力， 即使处于保护气氛 中， 压型模具表面膜层依然容易被氧化、 侵蚀。 高精密的模具是光学玻璃 精密模压工序中主要成本来源， 模具使用达不到一定的压型次数， 就不能 实现低成本、 高量产率的目的。 为延长模具寿命， 抑制高温环境对成型模 的损伤， 希望尽可能降低压型温度， 因此， 要求玻璃材料的转变温度（Tg) 和软化温度 （Ts ) 尽可能低。 确 认 本 用于非球面透镜的光学玻璃， 要求具有各种光学常数的玻璃， Nd 为 1. 77— 1. 84， Vd为 36— 44的光学玻璃在现代高级成像设备中应用较多， 含有铅、 钍的该类光学玻璃因对环境有害已不生产和使用， 不含铅、 钍的 该类光学玻璃通常为 B203 (Si02) — La203— Nb205 (Ta205) 一 RO ( R代表碱 土金属） 体系， 玻璃的软化温度通常远高于 600°C， 不适合用于精密模压。 In precision molding, in order to reproduce a high-precision die face on a glass molded article, it is necessary to press-form the glass preform at a high temperature (usually 15-4 CTC above the glass softening point temperature), at which time the molding die is exposed. At high temperatures and at a higher pressure, even in a protective atmosphere, the surface layer of the stamper is easily oxidized and eroded. The high-precision mold is the main cost source in the precision molding process of optical glass. If the mold does not reach a certain number of presses, the low-cost and high-volume yield cannot be achieved. In order to prolong the life of the mold and suppress damage to the molding die in a high temperature environment, it is desirable to lower the molding temperature as much as possible. Therefore, the transition temperature (Tg) and softening temperature (Ts) of the glass material are required to be as low as possible. Confirmation Optical glass for aspherical lenses, glass with various optical constants, optical glass with Nd of 1.77- 1.84, Vd of 36-44 is used in modern advanced imaging equipment, including lead and antimony. Such optical glass is not produced and used because it is harmful to the environment. The optical glass containing no lead or antimony is usually B 2 0 3 (Si0 2 ) — La 2 0 3 — Nb 2 0 5 (Ta 2 0 5 ) A RO (R stands for alkaline earth metal) system, the softening temperature of glass is usually much higher than 600 ° C, not suitable for precision molding.
美国专利 USP20030032542 公开了一种 B203 ( Si02) — La203— Gd203— Nb205— Zr02体系的光学玻璃， 该玻璃折射率在 1. 80以上， 阿贝数在 40左 右， 但玻璃的转变温度在 650°C以上， 不适合做精密模压材料。 中国专利 02155831. 0公开了一种 B203— Si02— La203^Gd203— ZnO— Li20组成的光学 玻璃系统， 但玻璃的阿贝数难以达到 43以下， 且从其实施例看， 玻璃成份 中含有较多含量的价格昂贵的 Ta205， 玻璃成本较高， 降低了产品竞争力。 日本特幵平 06—305769 公开了一种 Si02- B203- La203- Ta205- ZnO- Li20系统 精密压型用光学玻璃， 该系统玻璃同样使用较多的 Ta205， 且玻璃的液相温 度较高， 不利于批量化生产。 日本特开平 2002— 362938 公开了一种 B203 一 Si02—La203— ZnO~Nb205— Ta205— W03系统以及特开平 2002—012443 公 开的 B203- Si02- La203- Li20- ZnO- Nb205- Ta205- W03系统，虽然能达到较低的软 化温度， 但都使用了一定量的 Ta205， 玻璃成本昂贵。 U.S. Patent No. 2,003,032, 542 discloses an optical glass of a B 2 0 3 (Si0 2 ) — La 2 0 3 — Gd 2 0 3 — Nb 2 0 5 — Zr0 2 system having a refractive index of 1.80 or more, Abbe The number is around 40, but the glass transition temperature is above 650 ° C, which is not suitable for precision molding materials. Chinese Patent No. 02155831. 0 discloses an optical glass system composed of B 2 0 3 — Si0 2 — La 2 0 3 ^ Gd 2 0 3 — ZnO—Li 2 0, but the Abbe number of the glass is difficult to reach 43 or less, and From the examples, the glass component contains a large amount of expensive Ta 2 0 5 , and the glass cost is high, which reduces the competitiveness of the product. Japanese Patent Publication No. 06-305769 discloses an optical glass for precision molding of a Si0 2 - B 2 0 3 - La 2 0 3 - Ta 2 0 5 - ZnO- Li 2 0 system, which is also used in a large amount of glass. Ta 2 0 5 , and the liquidus temperature of the glass is high, which is not conducive to mass production. Japanese Patent Laid-Open No. 2002-362938 discloses a B 2 0 3 -Si0 2 -La 2 0 3 - ZnO~Nb 2 0 5 - Ta 2 0 5 - W0 3 system and a B 2 0 3 disclosed in Japanese Laid-Open Patent Publication No. 2002-012443 - Si0 2 - La 2 0 3 - Li 2 0- ZnO- Nb 2 0 5 - Ta 2 0 5 - W0 3 system, although a lower softening temperature can be achieved, a certain amount of Ta 2 0 5 is used , Glass is expensive.
发明内容 Summary of the invention
本发明所要解决的技术问题是提供一种高折射率低色散精密压型用 光学玻璃， 该光学玻璃不含铅、 砷、 镉等对环境有害物质， 不含有价格昂 贵的 Ta205， 玻璃软化温度满足精密模压要求。 The technical problem to be solved by the present invention is to provide an optical glass for high refractive index and low dispersion precision molding, which is free from environmentally harmful substances such as lead, arsenic and cadmium, and does not contain expensive Ta 2 0 5 , glass. The softening temperature meets the requirements for precision molding.
本发明解决技术问题所采用的技术方案是： 高折射率低色散精密压型 用光学玻璃， 其重量百分比组成为： Si02: 1—8%, B203: 16— 30%、 La203: 15— 40%、 Gd203: 0—20%、 ZnO: 8—30%、 Nb205 : 0. 5—14. 5%、 W03: 0—12. 5% 、 Ti02: 0—9%、 Li20: 0. 5—4%、 Zr02: 1—10%、 Y203 : 0—5%、 Yb203 : 0—5%, Lu203: 0—5%、 Na20: 0—3%、 K20: 0—2%、 A1203: 0—2%、 BaO: 0—3%、 CaO: 0—3%、 SrO: 0—3%、 MgO: 0—3%, Sb203 : 0— 0. 5%和 Sn02 : 0—0. 5%。 The technical solution adopted by the present invention to solve the technical problem is as follows: The optical glass for high refractive index and low dispersion precision molding has a weight percentage composition of: Si0 2 : 1-8%, B 2 0 3 : 16-30%, La 2 0 3 : 15—40%, Gd 2 0 3 : 0—20%, ZnO: 8—30%, Nb 2 0 5 : 0. 5—14. 5%, W0 3 : 0—12. 5%, Ti0 2 : 0-9%, Li 2 0: 0.5- 4%, Zr0 2 : 1 - 10%, Y 2 0 3 : 0-5%, Yb 2 0 3 : 0-5%, Lu 2 0 3 : 0—5%, Na 2 0: 0—3%, K 2 0: 0—2%, A1 2 0 3 : 0—2%, BaO: 0—3%, CaO: 0—3%, SrO: 0—3%, MgO: 0—3%, Sb 2 0 3 : 0—0. 5% and Sn0 2 : 0—0. 5%.
本发明的有益效果是： 本发明采用 B203_Si02— La203 (Gd203 ) 一 ZnO 系统， 使用合理比例的 Nb205、 W03、 Ti02使玻璃达到所需要的光学常数且具 有适于精密压型的良好物理化学特性。 本发明的光学玻璃转变温度 （Tg) 低于 560°C， 组份中不含有高价格的 Ta205， 同时玻璃具有良好的化学稳定 性， 能在单坩埚或连续熔炼池炉等设备上批量稳定生产， 适于低成本精密 模压成型非球面透镜等光学元件。 The beneficial effects of the present invention are as follows: The present invention adopts a B 2 0 3 _Si0 2 — La 2 0 3 (Gd 2 0 3 )-ZnO system, and uses a reasonable ratio of Nb 2 0 5 , W0 3 , Ti0 2 to achieve the desired glass. Optical constant Good physicochemical properties for precision molding. The optical glass transition temperature (Tg) of the present invention is lower than 560 ° C, and the composition does not contain high-priced Ta 2 0 5 , and the glass has good chemical stability and can be used in equipment such as single crucible or continuous melting furnace. Stable production in batches, suitable for low-cost precision molding of optical components such as aspherical lenses.
具体实施方式 detailed description
根据实验确定上述组份的重量百分比范围， 对上述各成份的作用及范 围限定的理由叙述如下。  The range of weight percentages of the above components is determined experimentally, and the reasons for the effects and ranges of the above components are described below.
B203是玻璃网络生成体氧化物， 是构成玻璃网络的必须成份， 尤其是 在高折射率的镧系玻璃中， B203是得到稳定玻璃的主要成份。 当 B203含量 低于 16%时， 玻璃的熔化性能变坏， 耐失透性能不理想； 当 03含量高于 30%, 玻璃的折射率达不到设计目标， 因此 B203的优选含量（重量百分比含 量， 以下同） 为 16%— 30%， 更优选含量为 19一 26%。 B 2 0 3 is a glass network-forming body oxide and is an essential component of a glass network. Especially in a high refractive index lanthanum glass, B 2 0 3 is a main component for obtaining a stable glass. When the content of B 2 0 3 is less than 16%, the melting property of the glass is deteriorated, and the devitrification resistance is not satisfactory; when the content of 0 3 is higher than 30%, the refractive index of the glass does not reach the design goal, so B 2 0 3 The preferred content (weight percent content, hereinafter the same) is from 16% to 30%, more preferably from 19% to 26%.
5102也是形成玻璃的网络生成体氧化物， 加入一定量的 Si02， 可增大玻 璃的高温粘度， 提高玻璃的耐失透性及化学稳定性。 当其含量不足 1%时， 玻璃的生产工艺性能差， 即前述作用不明显， 若超过 8%玻璃折射率下降， 耐失透性变差， 同时生产时原料熔化困难， 因此 Si02含量优选为 1一 8%， 更优选含量为 1一 6%。 510 2 is also a network-forming body oxide for forming glass. By adding a certain amount of Si0 2 , the high-temperature viscosity of the glass can be increased, and the devitrification resistance and chemical stability of the glass can be improved. When the content is less than 1%, the production process performance of the glass is poor, that is, the aforementioned effect is not obvious. If the refractive index of the glass exceeds 8%, the devitrification resistance is deteriorated, and at the same time, the raw material is difficult to be melted during production, so the SiO 2 content is preferably 1 to 8%, more preferably 1 to 6%.
La203是高折射低色散镧系光学玻璃的主要成份， 用于增加玻璃的折射 率且不会明显提高玻璃的色散， 在本发明中与 B203混合存在时可提高玻璃 的耐失透性能， 改善玻璃的化学稳定性。 当 La203含量小于 15%时， 不能获 得上述作用， 当其含量超过 40%时， 玻璃的析晶性能恶化， 因此 La203含量 优选为 15— 40%。 La 2 0 3 is a main component of the high-refraction low-dispersion lanthanide optical glass, and is used for increasing the refractive index of the glass without significantly increasing the dispersion of the glass. In the present invention, when mixed with B 2 0 3 , the glass resistance can be improved. Devitrification properties improve the chemical stability of the glass. When the content of La 2 O 3 is less than 15%, the above effects are not obtained, and when the content exceeds 40%, the devitrification property of the glass is deteriorated, so the La 2 O 3 content is preferably 15 to 40%.
Gd203的作用与 La203类似， 也是增加玻璃的折射率且不会明显提高玻 璃的色散， 在物理化学性能上起到改善玻璃化学稳定性和耐失透能力的作 用。 使用一定量的 Gd203代替 La203， 可以适当提高玻璃的耐失透能力， 但 可引起玻璃比重的增大。当 Gd203含量高于 20%时，玻璃的耐失透能力恶化， 因此 Gd203的含量优选为 0— 20%， 更优选为 5—15%。 The effect of Gd 2 0 3 is similar to that of La 2 0 3 , which also increases the refractive index of the glass and does not significantly increase the dispersion of the glass, and has the effect of improving the chemical stability and devitrification resistance of the glass in physical and chemical properties. By using a certain amount of Gd 2 0 3 instead of La 2 0 3 , the devitrification resistance of the glass can be appropriately increased, but the specific gravity of the glass can be increased. When the Gd 2 0 3 content is more than 20%, the devitrification resistance of the glass is deteriorated, so the content of Gd 2 0 3 is preferably from 0 to 20%, more preferably from 5 to 15%.
在本发明中， 为保证玻璃的高折射率低色散光学性能， 要求 La203和 Gd7( ^的总含量不少于 20%， 但当 LaA和 Gd，0;的总含量高于 45%时， 玻璃 的稳定性变差， 耐失透能力下降， 软化温度急剧升高， 因此 La203和 Gd203 的总含量优选为 20— 45%。 In the present invention, in order to ensure high refractive index and low dispersion optical properties of the glass, La 2 0 3 and Gd 7 (the total content of ^ is not less than 20%, but when the total content of LaA and Gd, 0; %, glass The stability is deteriorated, the devitrification resistance is lowered, and the softening temperature is sharply increased, so the total content of La 2 O 3 and Gd 2 0 3 is preferably 20 to 45%.
ZnO 是本发明玻璃的必须成份， 有利于降低玻璃的熔化温度和软化温 度， 并有调整玻璃光学性能的作用。 当其含量不足 8%时， 玻璃的软化温度 上升； 而当其含量高于 30%时， 玻璃的色散增大， 析晶倾向增大， 同时玻 璃的高温粘度变小， 给玻璃成型带来很大困难， 因此 ZnO的含量优选为 8 —30%, 更优选为 12— 28%。  ZnO is an essential component of the glass of the present invention, which is advantageous for lowering the melting temperature and softening temperature of the glass, and for adjusting the optical properties of the glass. When the content is less than 8%, the softening temperature of the glass increases; and when the content is more than 30%, the dispersion of the glass increases, the crystallization tendency increases, and the high temperature viscosity of the glass becomes small, which brings about a great glass forming. It is difficult, so the content of ZnO is preferably from 8 to 30%, more preferably from 12 to 28%.
Nb205是提高玻璃折射率的有效成份， 当其含量不到 0. 5%时， 玻璃的折 射率达不到设计目标， 而当其含量高于 14. 5%时， 会导致玻璃软化温度升 高， 同时使玻璃的透过率大幅下降， 因此 Nb205的含量优选为 0. 5—14. 5%。 Nb 2 0 5 is an effective component for increasing the refractive index of the glass. When the content is less than 0.5%, the refractive index of the glass does not reach the design goal, and when the content is higher than 14.5%, the glass softens. 5至14. 5%。 The content of the Nb 2 0 5 is preferably 0. 5-14. 5%.
W03具有提高玻璃折射率和色散以及改善玻璃析晶性能的作用，但实验 表明当其含量超过 12. 5%时， 玻璃的耐失透能力反而降低， 所以 W03的优选 含量为 0— 12. 5%， 更优选含量 0— 8%。 W0 3 has the effect of increasing the refractive index and dispersion of the glass and improving the crystallization property of the glass. However, the experiment shows that when the content exceeds 12.5%, the devitrification resistance of the glass is decreased, so the preferred content of W0 3 is 0-12. 5%, more preferably 0-8%.
Ti02对于提高玻璃的折射率和色散很有效， 并能提高玻璃的耐水性， 降低玻璃比重， 在本发明中， Ti02还起到增大玻璃高温粘度以改善玻璃析 晶性能的作用。 但其含量过高会造成玻璃着色。 因此 Ti02含量优选为 0— 9%。 - 上述 Nb205 、 W03和 Ti02的含量之和为 6. 5— 24%。 Ti0 2 is effective for increasing the refractive index and dispersion of the glass, and can improve the water resistance of the glass and lower the specific gravity of the glass. In the present invention, Ti0 2 also functions to increase the high temperature viscosity of the glass to improve the crystallization property of the glass. However, if the content is too high, the glass will be colored. Therefore, the Ti0 2 content is preferably from 0 to 9%. 5至24百分比。 The sum of the content of the above Nb 2 0 5 , W0 3 and Ti0 2 is 6.5 - 24%.
Li20是降低玻璃的转变温度和软化温度的最有效成份， Li20还有较强 助熔作用。 当其含量低于 0. 5%时， 对降低转变温度效果不明显； 但当含量 高于 4%时， 玻璃的耐失透性急剧下降， 因此 Li20的优选含量为 0. 5— 4%， 更优选含量为 0. 5— 3%。 Li 2 0 is the most effective component for lowering the transition temperature and softening temperature of the glass, and Li 2 0 has a stronger fluxing effect. 5 - 4 The preferred content of Li 2 0 is 0. 5 — 4 The preferred content of Li 2 0 is 0. 5— 4 5至3%。 The %, more preferably 0. 5 - 3%.
Ζι 2具有改善玻璃耐失透性、提高化学稳定性的效果， 在镧系玻璃中， 还起到提高折射率降低色散的作用。但其含量低于 1%时，起不到上述作用； 当其含量高于 10%时， 引起玻璃软化温度上升， 同时玻璃耐失透性恶化。 因此 Zr02的优选含量为 1一 10%。 Ζι 2 has an effect of improving the resistance to devitrification of the glass and improving the chemical stability, and also serves to increase the refractive index and reduce the dispersion in the bismuth-based glass. However, when the content is less than 1%, the above effect is not obtained; when the content is more than 10%, the glass softening temperature is increased, and the glass resistance to devitrification is deteriorated. Therefore, the preferred content of Zr0 2 is from 1 to 10%.
Y203、 Yb203和 Lu203具有提高玻璃稳定性和耐失透性能的作用， 还可以 调整玻璃的光学常数， 但当含量超过 5%， 会引起玻璃转变温度升高， 因此 Y203优选含量为 0— 5%， 更优选不加入； Yb203优选含量为 0— 5%， 更优选不 加入； Lu203优选含量为 0— 5%， 更优选不加入。 Y 2 0 3 , Yb 2 0 3 and Lu 2 0 3 have the effects of improving glass stability and devitrification resistance, and can also adjust the optical constant of the glass, but when the content exceeds 5%, the glass transition temperature is increased. Therefore, Y 2 0 3 is preferably present in an amount of from 0 to 5%, more preferably not added; Yb 2 0 3 is preferably present in an amount of from 0 to 5%, more preferably not Addition; Lu 2 0 3 is preferably present in an amount of from 0 to 5%, more preferably not added.
Na20具有降低玻璃转变温度， 提高玻璃透明度的作用， 但当其含量超 过 3%， 会增大玻璃的析晶倾向， 同时显著降低玻璃的折射率， 因此 Ν 0优 选含量为 0— 3%， 更优选含量为 0— 1%。 Na 2 0 has the effect of lowering the glass transition temperature and increasing the transparency of the glass. However, when the content exceeds 3%, the crystallization tendency of the glass is increased, and the refractive index of the glass is remarkably lowered. Therefore, the content of Ν 0 is preferably 0 to 3%. More preferably, the content is 0-1%.
Κ20的作用与 Na20类似， 其优选含量为 0— 2%， 更优选不加入。 The effect of Κ 20 is similar to that of Na 2 0, and its preferred content is 0 to 2%, more preferably not added.
A1203可以提高玻璃的化学稳定性， 增大玻璃高温粘度， 但当其含量高 于 2%， 会引起玻璃的耐失透性下降， 增加熔融难度。 因此 A1203优选为 0 —2%, 更优选不加入。 A1 2 0 3 can improve the chemical stability of the glass and increase the high temperature viscosity of the glass. However, when the content is higher than 2%, the devitrification resistance of the glass is lowered, and the melting difficulty is increased. Therefore, A1 2 0 3 is preferably 0 - 2%, more preferably not added.
BaO可以降低玻璃的色散， 同时改善玻璃的透过率。但当含量超过 3%， 不能达到玻璃的折射率目标， 同时会增大玻璃的析晶倾向。 因此 BaO优选 法含量为 0— 3%。  BaO can reduce the dispersion of the glass while improving the transmittance of the glass. However, when the content exceeds 3%, the refractive index target of the glass cannot be achieved, and the crystallization tendency of the glass is increased. Therefore, the BaO preferably has a content of from 0 to 3%.
CaO可以提高玻璃的化学稳定性， 并有助熔作用， 但其含量高于 3%时 玻璃的析晶倾向增大。 因此 CaO优选含量为 0— 3%， 更优选不加入。  CaO can improve the chemical stability of the glass and has a fluxing effect, but when the content is higher than 3%, the crystallization tendency of the glass increases. Therefore, CaO is preferably contained in an amount of from 0 to 3%, more preferably not added.
MgO和 SrO的作用与 CaO类似， 可以提高玻璃的均质性。 MgO优选含量 为 0— 3%， 更优选不加入； SrO优选含量为 0— 3%， 更优选不加入。  The action of MgO and SrO is similar to that of CaO, which improves the homogeneity of the glass. The MgO content is preferably from 0 to 3%, more preferably not added; and the SrO is preferably from 0 to 3%, more preferably not added.
Sb203和 Sn02作为除泡剂使用， Sb203优选含量为 0— 0. 5%， 更优选不加 入； Sn02优选含量为 0— 0. 5%， 更优选不加入。 Sb 2 0 3 and Sn0 2 are used as a defoaming agent, and the content of Sb 2 0 3 is preferably 0-0.5%, more preferably not added; and the content of Sn0 2 is preferably 0-0.5%, more preferably not added.
考虑对环境无污染， 本发明不使用 Pb0、 As203和 CdO等成份。 Considering that the environment is not polluted, the present invention does not use components such as Pb0, As 2 0 3 and CdO.
本发明的生产方法是：  The production method of the present invention is:
将组成成份对应的氧化物、 氢氧化物、 碳酸盐、 硝酸盐原料， 按比例 称量， 充分混合后加入铂金坩埚或连续熔炼池炉内， 在 1240— 132CTC下熔 化、 澄清和均化后降温， 将熔融玻璃液浇注到预热后的金属模具内， 将玻 璃连同金属模一起放入退火炉内， 徐冷退火后即得。  The oxide, hydroxide, carbonate, and nitrate raw materials corresponding to the composition are weighed in proportion, thoroughly mixed, added to a platinum crucible or a continuous melting furnace, and melted, clarified, and homogenized at 1240-132 CTC. After cooling, the molten glass liquid is poured into the preheated metal mold, and the glass is placed in the annealing furnace together with the metal mold, and is obtained by quenching and annealing.
以下是本发明的实施例， 但本发明并不受这些实施例的限制。  The following are examples of the invention, but the invention is not limited by the examples.
实施例： 1一 24  Example: 1-24
表 1、 表 2、 表 3和表 4列出了本发明的 24个实施例和 3个比较例， 表中列出了玻璃的折射率 （Nd )、 阿贝数 （Vd )、 转变温度 （Tg)、 密度 （d ) 以及透过率为 80%和 5%的波长比 （分别用 λ 80、 λ 5表示）。 9 Table 1, Table 2, Table 3 and Table 4 list 24 examples and 3 comparative examples of the present invention, which list the refractive index (Nd), Abbe number (Vd), and transition temperature of the glass ( Tg), density (d), and transmittance ratios of 80% and 5% (expressed by λ 80 and λ 5 , respectively). 9
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U6Z00/L00Z l3/13d 00£9讀 OOZ OAV 组份 实施例 比较例 U6Z00/L00Z l3/13d 00£9 read OOZ OAV Component Example Comparative Example
22 23 24 1 2 3  22 23 24 1 2 3
Si02 1.0 5.0 4.0 3.0 7.0 Si0 2 1.0 5.0 4.0 3.0 7.0
B203 30.0 22.0 20.6 30.0 22.0 21.0 B 2 0 3 30.0 22.0 20.6 30.0 22.0 21.0
La203 26.0 15.6 32.0 35.0 32.0 27.0 La 2 0 3 26.0 15.6 32.0 35.0 32.0 27.0
Gd203 9.8 20 2.0 Gd 2 0 3 9.8 20 2.0
ZnO 16.0 20.0 30.0 5.2 23.0 19.0  ZnO 16.0 20.0 30.0 5.2 23.0 19.0
Nb205 9.0 7.0 6.0 17.0 6.0 8.0 Nb 2 0 5 9.0 7.0 6.0 17.0 6.0 8.0
W03 3.0 5.1 1.3 5.0 5.9 6.0 W0 3 3.0 5.1 1.3 5.0 5.9 6.0
Ti02 1.0 1.1 3.5 Ti0 2 1.0 1.1 3.5
Li20 1.2 1.3 0.5 1.3 1.0 1.0 Li 2 0 1.2 1.3 0.5 1.3 1.0 1.0
Zr02 3.0 4.0 2.5 3.5 2.0 1.5 Zr0 2 3.0 4.0 2.5 3.5 2.0 1.5
Ta205 5.0 5.0 Ta 2 0 5 5.0 5.0
CaO  CaO
Y2O3 0.5  Y2O3 0.5
Yb203 3.0 Yb 2 0 3 3.0
Lu203 Lu 2 0 3
AI2O3  AI2O3
SrO  SrO
BaO  BaO
Na20 Na 2 0
K20 K 2 0
MgO  MgO
Sn02 Sn0 2
Sb203 0.1 0.5 Sb 2 0 3 0.1 0.5
Nd 1.7712 1.7833 1.8126 1.8187 1.8059 1.8120  Nd 1.7712 1.7833 1.8126 1.8187 1.8059 1.8120
Vd 40.6 40.2 40.1 38.5 40.5 36.7  Vd 40.6 40.2 40.1 38.5 40.5 36.7
Tg (°C) 550 540 550 595 535 575  Tg (°C) 550 540 550 595 535 575
d (g/cmJ) 4.45 4.48 4.42 4.52 4.50 4.50 d (g/cm J ) 4.45 4.48 4.42 4.52 4.50 4.50
入 80/入 5 40/34 39/34 40/34 41/35 39/34 42/35  80/in 5 40/34 39/34 40/34 41/35 39/34 42/35
表 4  Table 4
从以上实施例可以看出：本发明光学玻璃的折射率 (Nd)为 1.77— 1.84， 阿贝数 （Vd) 为 35— 43， 玻璃转变温度不超过 560Ό, 化学稳定性优异， 耐失透性及着色度良好， 比重小， 非常适于精密模压成型非球面透镜、 球 面透镜等光学元件， 并且玻璃组份中不含有价格昂贵的 Τ 05原料， 成本低 廉， 具有市场竞争优势。 It can be seen from the above examples that the refractive index (Nd) of the optical glass of the present invention is 1.77 - 1.84, the Abbe number (Vd) is 35 - 43, the glass transition temperature does not exceed 560 Å, the chemical stability is excellent, and the devitrification resistance is obtained. and a good degree of coloring, the proportion of small, very suitable for precision press molding an optical element aspherical lens, a spherical lens or the like, and does not contain glass components Τ 0 5 expensive raw materials, low cost, has a competitive advantage.

Claims

权 利 要 求 书 Claim
1、 高折射率低色散精密压型用光学玻璃， 其特征在于： 其重量百分比 组成为： Si02: 1一 8%、 B203: 16— 30%、 La203: 15—40%、 Gd203: 0—20%、 ZnO: 8—30%、 Nb205: 0.5—14.5%、 W03: 0—12.5% 、 Ti02: 0—9%、 Li20: 0.5—4%、 Zr02: 1—10%、 Y203: 0—5%、 Yb203: 0—5%、 Lu203: 0—5%、 Na20: 0— 3%、 20: 0—2%. A1203: 0—2%、 BaO: 0—3%、 CaO: 0—3%、 SrO: 0— 3%、 MgO: 0—3%、 Sb203: 0—0.5%和 Sn02: 0—0.5%。 1. Optical glass for high refractive index and low dispersion precision molding, characterized in that the composition by weight is: Si0 2 : 1 - 8%, B 2 0 3 : 16 - 30%, La 2 0 3 : 15 - 40 %, Gd 2 0 3: 0-20%, ZnO: 8-30%, Nb 2 0 5 : 0.5-14.5%, W0 3: 0-12.5%, Ti0 2: 0-9%, Li 2 0: 0.5 —4%, Zr0 2 : 1—10%, Y 2 0 3: 0—5%, Yb 2 0 3: 0—5%, Lu 2 0 3: 0—5%, Na 2 0: 0—3% 2 0: 0-2%. A1 2 0 3 : 0-2%, BaO: 0-3%, CaO: 0-3%, SrO: 0-3%, MgO: 0-3%, Sb 2 0 3 : 0-0.5% and Sn0 2: 0-0.5%.
2、 如权利要求 1所述的高折射率低色散精密压型用光学玻璃， 其特征 在于： 其重量百分比组成为： Si02: 1—6%, B203: 19一 26%、 La203: 15— 40%、 Gd203: 5—15%、 ZnO: 12—28%、 Nb205: 0.5—14.5%、 W03: 0—8% 、 Ti02: 0—9%、 Li20: 0.5—3%、 Zr02: 1—10%、 Na20: 0—1%和 BaO: 0—3%。 The optical glass for high refractive index low dispersion precision molding according to claim 1, wherein the weight percentage composition is: Si0 2 : 1 - 6%, B 2 0 3 : 19 - 26%, La 2 0 3 : 15-40%, Gd 2 0 3 : 5-15%, ZnO: 12-28%, Nb 2 0 5: 0.5-14.5%, W0 3: 0-8%, Ti0 2: 0-9 %, Li 2 0: 0.5-3%, Zr0 2 : 1 - 10%, Na 2 0: 0 - 1%, and BaO: 0 - 3%.
3、 如权利要求 1或 2所述的高折射率低色散精密压型用光学玻璃， 其 特征在于： 所述 1^203和 Gd203的重量百分比之和为 20— 45%。 The optical glass for high refractive index low dispersion precision molding according to claim 1 or 2, wherein the sum of the weight percentages of the 1 2 2 3 3 and the Gd 2 0 3 is 20 to 45%.
4、 如权利要求 1或 2所述的高折射率低色散精密压型用光学玻璃， 其 特征在于： 所述 Nb205 、 W03和 Ti02的重量百分比之和为 6.5— 24%。 The optical glass for high refractive index low dispersion precision molding according to claim 1 or 2, wherein the sum of the weight percentages of the Nb 2 0 5 , W0 3 and Ti0 2 is 6.5 to 24%.
5、 根据权利要求 1或 2所述的高折射率低色散精密压型用光学玻璃， 其特征在于： 所述光学玻璃的转变温度不超过 560Ό。  The optical glass for high refractive index low dispersion precision molding according to claim 1 or 2, wherein the optical glass has a transition temperature of not more than 560 Å.
PCT/CN2007/002921 2006-10-17 2007-10-11 High-refractivity low-dispersion optical glass for precise press molding WO2008046300A1 (en)

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