CN116177872A - Optical glass, glass preform, optical element, and optical instrument - Google Patents
Optical glass, glass preform, optical element, and optical instrument Download PDFInfo
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- CN116177872A CN116177872A CN202310276821.7A CN202310276821A CN116177872A CN 116177872 A CN116177872 A CN 116177872A CN 202310276821 A CN202310276821 A CN 202310276821A CN 116177872 A CN116177872 A CN 116177872A
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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
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
The invention provides optical glass, which comprises the following components in percentage by weight: siO (SiO) 2 ：3～20％；B 2 O 3 ：8～30％；La 2 O 3 ：8～25％；Nb 2 O 5 : 15-43%; baO:1 to 15 percent of Nb 2 O 5 /La 2 O 3 0.8 to 3.0. Through reasonable component design, the optical glass obtained by the invention has the expected refractive index and Abbe number, and meanwhile, the density of the glass is lower, so that greater freedom is brought for realizing light weight of an optical system; has excellent chemical stability and crystallization resistance, can not obviously reduce the transmittance after long-term use, is well suited for use in imaging applications where a harsh operating environment is required.
Description
The present application is a divisional application of the invention patent application with the application number 201911309339.9 and the application date 2019, 12 month and 18 date, named "optical glass, glass preform, optical element and optical instrument".
Technical Field
The invention relates to optical glass, in particular to lanthanum-containing optical glass with a refractive index of 1.82-1.90 and an Abbe number of 27-35.
Background
In the prior art, glass with a refractive index of 1.82-1.90 and an Abbe number of 27-35 belongs to high-refractive-index glass, and is widely applied to various lens designs. In recent years, there has been a demand for weight reduction of optical elements such as lenses, and particularly in aerial photography using a small-sized remote operation machine such as an unmanned aerial vehicle, there has been a demand for not only weight reduction but also chemical stability of an optical system to be able to cope with a severe environment.
However, in the glass formulation system of the same system, the density and chemical stability of the glass are closely related to the glass structure. The more loose the glass structure, the less dense the glass, and also means that the chemical stability of the glass is reduced. How to reduce the density of glass and ensure the chemical stability of the glass at the same time, so that the glass has more advantages in application, which is a new subject developed in the era for optical design and optical material research.
In the prior art, the optical glass with the refractive index of 1.82-1.90 and Abbe number of 27-35 has the density value of basically 4.2g/cm 3 As described above, if the density is lower than 4.2g/cm, the density can be developed as shown in Table 1 below 3 Even below 4.00g/cm 3 The heavy lanthanum flint glass with the above gloss can effectively solve the problem of light weight in design.
Table 1: density and chemical stability of partially lanthanum containing optical glass
The heavy lanthanum flint glass with the refractive index and Abbe number can reach the temperature lower than 4.0g/cm if required 3 The density of the glass is different from the conventional density in component design, and the problems of poor crystallization resistance, difficult elimination of streak bubbles and the like are usually brought to the glass. If the crystallization resistance of the glass is poor, firstly, the production difficulty of the glass blank is increased, the yield is reduced, and even normal production cannot be carried out when the yield is severe; secondly, crystals are easy to be separated out in the secondary pressing process, so that the yield is reduced, and even the secondary pressing cannot be performed. For glass materials used in the automotive field, if glassThe production yield is low, and the production cannot be carried out by adopting a secondary pressing method but a cold working method, so that the cost is greatly increased.
Disclosure of Invention
The invention aims to provide optical glass with low density, excellent chemical stability and crystallization resistance.
The technical scheme adopted for solving the technical problems is as follows:
(1) The optical glass comprises the following components in percentage by weight: siO (SiO) 2 ：2～20％；B 2 O 3 ：8～30％；La 2 O 3 ：8～25％；Nb 2 O 5 : 15-43%; baO:1 to 15 percent of Nb 2 O 5 /La 2 O 3 0.8 to 3.0.
(2) The optical glass according to (1), which comprises the following components in percentage by weight: gd (Gd) 2 O 3 ：0～8％；Y 2 O 3 ：0～5％；Al 2 O 3 ：0～3％；TiO 2 ：0～9％；ZrO 2 ：0～8％；ZnO：0～7％；MgO：0～5％；CaO：0～23％；SrO：0～5％；Li 2 O：0～5％；K 2 O：0～5％；Na 2 O: 0-5%; clarifying agent: 0 to 1 percent.
(3) The optical glass comprises the following components in percentage by weight 2 ：2～20％；B 2 O 3 ：8～30％；La 2 O 3 ：8～25％；Nb 2 O 5 ：15～43％；BaO：1～15％；Gd 2 O 3 ：0～8％；Y 2 O 3 ：0～5％；Al 2 O 3 ：0～3％；TiO 2 ：0～9％；ZrO 2 ：0～8％；ZnO：0～7％；MgO：0～5％；CaO：0～23％；SrO：0～5％；Li 2 O：0～5％；K 2 O：0～5％；Na 2 O: 0-5%; clarifying agent: 0 to 1%, wherein Nb 2 O 5 /La 2 O 3 0.8 to 3.0.
(4) Optical glass containing SiO 2 、B 2 O 3 、La 2 O 3 、Nb 2 O 5 And an alkaline earth metal oxide, the components of which are expressed in weight percent, wherein SiO 2 /B 2 O 3 0.1 to 1.2, nb 2 O 5 /La 2 O 3 0.8 to 3.0, and the refractive index n of the optical glass d Is 1.82 to 1.90, abbe number v d 27-35, density ρ of 4.2g/cm 3 The following is given.
(5) The optical glass according to (4), which comprises the following components in percentage by weight: siO (SiO) 2 : 2-20%; and/or B 2 O 3 : 8-30%; and/or La 2 O 3 : 8-25%; and/or Nb 2 O 5 : 15-43%; and/or BaO: 1-15%; and/or Gd 2 O 3 : 0-8%; and/or Y 2 O 3 : 0-5%; and/or Al 2 O 3 :0 to 3 percent; and/or TiO 2 : 0-9%; and/or ZrO 2 : 0-8%; and/or ZnO: 0-7%; and/or MgO: 0-5%; and/or CaO: 0-23%; and/or SrO: 0-5%; and/or Li 2 O: 0-5%; and/or K 2 O: 0-5%; and/or Na 2 O: 0-5%; and/or clarifying agent: 0 to 1 percent.
(6) The optical glass according to any one of (1) to (5), wherein the components are represented by weight percent: siO (SiO) 2 /B 2 O 3 From 0.1 to 1.2, preferably SiO 2 /B 2 O 3 From 0.12 to 1.0, more preferably SiO 2 /B 2 O 3 0.15 to 0.8.
(7) The optical glass according to any one of (1) to (5), wherein the components thereof are expressed in weight percent, satisfying one or more of the following 7 cases:
1)Nb 2 O 5 /La 2 O 3 1.0 to 2.8;
2)TiO 2 /Nb 2 O 5 is 0.5 or less;
3) CaO/(BaO+SrO) is 1.0 or less;
4)Li 2 O+K 2 O+Na 2 o is less than 5%;
5)Li 2 O/(K 2 O+Na 2 o) is 0.5 or less;
6)(BaO+SrO+CaO)/(La 2 O 3 +Gd 2 O 3 +Y 2 O 3 ) 0.4 to 2.0;
7)(CaO+BaO+SrO)/(Al 2 O 3 +ZrO 2 +TiO 2 ) The value of (2) is less than 3.0.
(8) The optical glass according to any one of (1) to (5), wherein the components are represented by weight percent: siO (SiO) 2 : 3-18%; and/or B 2 O 3 : 10-28%; and/or La 2 O 3 : 10-23%; and/or Nb 2 O 5 : 20-42%; and/or BaO: 4-13%; and/or Gd 2 O 3 :0 to 6 percent; and/or Y 2 O 3 :0 to 3 percent; and/or Al 2 O 3 :0 to 2 percent; and/or TiO 2 : 0.5-8%; and/or ZrO 2 :0.1 to 8 percent; and/or ZnO: 0-5%; and/or MgO:0 to 3 percent; and/or CaO: 0-20%; and/or SrO:0 to 4 percent; and/or Li 2 O:0 to 3 percent; and/or K 2 O:0 to 4 percent; and/or Na 2 O:0.1 to 5 percent; and/or clarifying agent: 0 to 0.5 percent.
(9) The optical glass according to any one of (1) to (5), wherein the components thereof are expressed in weight percent, satisfying one or more of the following 7 cases:
1)Nb 2 O 5 /La 2 O 3 1.2 to 2.6;
2)TiO 2 /Nb 2 O 5 is 0.4 or less;
3) CaO/(BaO+SrO) is 0.01-0.9;
4)Li 2 O+K 2 O+Na 2 o is below 4%;
5)Li 2 O/(K 2 O+Na 2 o) is 0.4 or less;
6)(BaO+SrO+CaO)/(La 2 O 3 +Gd 2 O 3 +Y 2 O 3 ) 0.5 to 1.8;
7)(CaO+BaO+SrO)/(Al 2 O 3 +ZrO 2 +TiO 2 ) The value of (2) is less than 2.8.
(10) The optical glass according to any one of (1) to (5), wherein the components are represented by weight percent: siO (SiO) 2 : 4-16%; and/or B 2 O 3 : 15-25%; and/or La 2 O 3 : 12-21%; and/or Nb 2 O 5 : 22-40%; and/or BaO: 5-12%; and/or Gd 2 O 3 :0 to 4 percent; and/or Y 2 O 3 :0 to 2 percent; and/or Al 2 O 3 :0 to 1 percent; and/or TiO 2 :1 to 5 percent; and/or ZrO 2 : 0.5-7%; and/or CaO: 2-15%; and/or SrO:0 to 3 percent; and/or K 2 O:0 to 3 percent; and/or Na 2 O:0.5 to 3 percent; and/or clarifying agent: 0 to 0.1 percent.
(11) The optical glass according to any one of (1) to (5), wherein the components thereof are expressed in weight percent, satisfying one or more of the following 6 cases:
1)TiO 2 /Nb 2 O 5 is 0.2 or less;
2) CaO/(BaO+SrO) is 0.02-0.8;
3)Li 2 O+K 2 O+Na 2 o is less than 3%;
4)Li 2 O/(K 2 O+Na 2 o) is 0.3 or less;
5)(BaO+SrO+CaO)/(La 2 O 3 +Gd 2 O 3 +Y 2 O 3 ) 0.7 to 1.5;
6)(CaO+BaO+SrO)/(Al 2 O 3 +ZrO 2 +TiO 2 ) The value of (2) is less than 2.5.
(12) The optical glass according to any one of (1) to (5), which has a refractive index n d 1.82 to 1.90, preferably 1.83 to 1.88, more preferably 1.84 to 1.87; abbe number v d 27 to 35, preferably 28 to 34, more preferably 28 to 32.
(13) The optical glass according to any one of (1) to (5), which has stability against water action D W Class 3 or more, preferably class 2 or more, more preferably class 1; and/or acid action resistance stability D A More than 3 kinds, preferablyClass 2 or more, more preferably class 1; and/or density ρ of 4.2g/cm 3 Hereinafter, it is preferably 4.0g/cm 3 Hereinafter, it is more preferably 3.9g/cm 3 Hereinafter, it is more preferably 3.8g/cm 3 The following are set forth; and/or the streak degree is C or more, preferably B or more, more preferably a.
(14) A glass preform made of the optical glass according to any one of (1) to (13).
(15) An optical element made of the optical glass according to any one of (1) to (13) or made of the glass preform according to (14).
(16) An optical device comprising the optical glass according to any one of (1) to (13) or the optical element according to (15).
The beneficial effects of the invention are as follows: through reasonable component design, the optical glass obtained by the invention has the expected refractive index and Abbe number, and meanwhile, the density of the glass is lower, so that greater freedom is brought for realizing light weight of an optical system; has excellent chemical stability and crystallization resistance, can not obviously reduce the transmittance after long-term use, is well suited for use in imaging applications where a harsh operating environment is required.
Detailed Description
The embodiments of the optical glass of the present invention will be described in detail below, but the present invention is not limited to the following embodiments, and can be implemented with appropriate modifications within the scope of the object of the present invention. In the repeated explanation, explanation is omitted appropriately, but the gist of the invention is not limited thereto. In the following, the optical glass of the present invention may be simply referred to as glass.
[ optical glass ]
The respective component ranges of the optical glass of the present invention are described below. In the present specification, unless otherwise specified, the contents of the respective components are all expressed in terms of weight percentage relative to the total amount of glass substance converted into the composition of oxide. The term "composition converted into oxide" as used herein means that the total amount of oxide used as a raw material of the optical glass composition (component) of the present invention is 100% based on the total amount of oxide when the oxide, composite salt, hydroxide, or the like is decomposed and converted into oxide in the melt.
Unless otherwise indicated in a particular context, numerical ranges set forth herein include upper and lower limits, and "above" and "below" include endpoints, and all integers and fractions within the range, and are not limited to the specific values set forth in the defined range. The term "and/or" as referred to herein is inclusive, e.g. "a; and/or B ", means either a alone, B alone, or both a and B.
The optical glass of the invention mainly contains SiO 2 、B 2 O 3 、La 2 O 3 、Nb 2 O 5 And RO (R0 is one or more than one of MgO, caO, srO, baO), and the optical glass obtained through reasonable component proportion has the expected refractive index and Abbe number, and meanwhile, the density of the glass is lower, so that the optical system is lighter and has larger degree of freedom; has excellent chemical stability and crystallization resistance, can not obviously reduce the transmittance after long-term use, is well suited for use in imaging applications where a harsh operating environment is required.
SiO 2 And B 2 O 3 The glass is a network forming body forming the glass, and the content of the network forming body is a basis for forming the glass, and is closely related to key indexes such as glass forming stability, crystallization resistance, refractive index, abbe number and the like of the glass. Wherein, if SiO 2 If the content exceeds 20%, the glass becomes difficult to melt, meanwhile, the glass forming stability is reduced, the crystallization resistance is rapidly reduced, and the refractive index and Abbe number of the glass cannot meet the design requirements; if SiO is 2 The content of (2) is lower than 2%, and the chemical stability of the glass, especially the stability against water action, is lowered. Thus, siO 2 The content of (2) to (20%), preferably 3% to (18%), more preferably 4% to (16%).
B 2 O 3 If the content exceeds 30%, the chemical stability of the glass is lowered, and the Abbe number is higher than the design expectation; b (B) 2 O 3 If the content of (2) is less than 8%, the stability of the glass is deteriorated, the crystallization resistance is rapidly reduced, and the Abbe number of the glass does not reach the design expectation. Because ofThis, B 2 O 3 The content of (2) is limited to 8 to 30%, preferably 10 to 28%, more preferably 15 to 25%.
The inventor has found through a great deal of experimental research that SiO 2 And B is connected with 2 O 3 To a certain extent, determines B 2 O 3 Structural state in glass, and B 2 O 3 The structural state of (2) has larger influence on two indexes of refractive index and chemical stability of glass, when SiO 2 And B is connected with 2 O 3 Ratio SiO of (2) 2 /B 2 O 3 When the refractive index of the glass is more than 1.2, the refractive index of the glass cannot meet the design requirement; if SiO is 2 /B 2 O 3 When the glass content is less than 0.1, the chemical stability of the glass is rapidly lowered, and the requirements for use in severe conditions cannot be satisfied. On the other hand, for production, if SiO 2 /B 2 O 3 The value of (2) is less than 0.1, the high-temperature viscosity of the glass is extremely small during forming, and fringes below C level are easily generated in the glass, so that the glass cannot be applied to an imaging system with high requirements. Thus, siO 2 /B 2 O 3 The value of (2) is 0.1 to 1.2, preferably 0.12 to 1.0, more preferably 0.15 to 0.8.
La 2 O 3 The glass is an important component of the glass, and the refractive index of the glass can be rapidly improved by adding the glass, so that the glass has the performance of high refractive index and high dispersion. However, if the content exceeds 25%, the crystallization resistance of the glass is drastically lowered; on the other hand, the inventors have found that, when La 2 O 3 When the content exceeds 25%, the density value of the glass can be rapidly increased, which is contrary to the aim of reducing the density value of the glass in the invention; if the content is less than 8%, the refractive index and dispersion of the glass do not meet the design requirements, and the chemical stability, particularly the water resistance, of the glass is reduced. Therefore La 2 O 3 The content of (2) is 8 to 25%, preferably 10 to 23%, more preferably 12 to 21%.
To at La 2 O 3 The inventors have found that the addition of a proper amount of Gd can maintain good crystallization resistance even when the content is relatively high 2 O 3 、Y 2 O 3 、ZrO 2 、TiO 2 、Al 2 O 3 One or more of the components can improve the crystallization resistance of the glass.
Gd 2 O 3 Effect on refractive index and dispersion and La 2 O 3 Similarly, if the content is higher than 8%, the refractive index temperature coefficient of the glass increases rapidly, the cost increases rapidly, and the crystallization resistance of the glass decreases adversely, so Gd 2 O 3 The content of (2) is limited to 0 to 8%, preferably 0 to 6%, more preferably 0 to 4%.
Proper amount of Y 2 O 3 Added into glass to replace La 2 O 3 The refractive index and dispersion of the glass are not greatly changed, but if the content exceeds 5%, the temperature coefficient of the refractive index of the glass is rapidly increased, and the crystallization resistance of the glass is reduced. Thus Y 2 O 3 The content of (2) is limited to 0 to 5%, preferably 0 to 3%, more preferably 0 to 2%.
ZrO 2 The glass can be added into the glass to improve the crystallization resistance of the glass and remarkably improve the chemical stability of the glass. More importantly, adding proper amount of ZrO 2 The corrosion of molten glass to refractory materials in the production process can be obviously reduced, on one hand, the service life of a furnace body can be prolonged, the maintenance cost and waste discharge of the furnace body are reduced, on the other hand, impurities in the refractory materials can be obviously inhibited from entering glass, and the transmittance and crystallization resistance stability of the glass are improved. However, zrO 2 In the case of the bulk glass, it is detrimental to lowering the temperature coefficient of refractive index of the glass, and if the content exceeds 8%, the temperature coefficient of refractive index of the glass is rapidly raised to fail to meet the design requirements, and at the same time, the glass becomes very difficult to melt, and the crystallization resistance is rapidly lowered, so that ZrO in the present invention 2 The content is limited to 8% or less. If ZrO 2 The content of (2) is less than 0.1%, and the erosion of the glass to the refractory material is obviously increased. Thus, zrO in the present invention 2 The content is preferably 0.1 to 8%, more preferably 0.5 to 7%, and even more preferably 1 to 6%.
Proper amount of Al 2 O 3 The anti-crystallization property of the glass can be improved by adding the glass into the glass, and meanwhileThe ability of the molten glass to corrode the crucible material can also be reduced. However, if the amount of the additive is more than 3%, the refractive index temperature coefficient of the glass increases, and at the same time, the melting property of the glass decreases, and the refractive index also decreases rapidly. Therefore, the content is limited to 3% or less, preferably 2% or less, and more preferably 1% or less.
Proper amount of TiO 2 The glass can be added into the glass, so that the sunlight resistance stability and crystallization resistance of the glass can be improved, and the density value of the glass can be reduced. But TiO 2 For bulk glass, it is detrimental to improve the degree of staining of the glass. Through a great number of experiments, the inventor finds that if the content exceeds 9%, the staining degree of the glass cannot meet the design requirement. Thus, in the present invention, tiO 2 The content is 0 to 9%, preferably 0.5 to 8%, more preferably 1 to 5%.
Nb 2 O 5 Belongs to a high-refraction high-dispersion component, and can be added into glass to adjust the refractive index and dispersion of the glass, reduce the density of the glass, improve the crystallization resistance of the glass and improve the stability of the glass. If Nb is 2 O 5 The Abbe number of the glass is rapidly decreased and the crystallization resistance of the glass is also rapidly decreased by exceeding 43%, thus Nb in the invention 2 O 5 The content of (2) is limited to 43% or less, preferably 42% or less, and more preferably 40% or less. If Nb is 2 O 5 If the content of (C) is less than 15%, then this means that more lanthanum oxide or other high dispersion oxide as described above needs to be added, which leads to a rapid increase in the density of the glass, and thus Nb 2 O 5 The lower limit of the content of (2) is 15%, preferably 20%, more preferably 22%.
Furthermore, the glass related to the invention can be exposed to sunlight for a long time when used in an outdoor severe environment, especially in a plateau area. Conventional optical glass is designed for photographic equipment, and the problem of reduced transmittance of the glass after long-term exposure is not generally considered. Therefore, how to improve the sunlight resistance stability of the glass is a key problem of the glass of the invention.
Through multiple experiments by the inventor, nb 2 O 5 And TiO 2 At the same time using TiO than singly using 2 The effect of improving the sunlight resistance stability of the glass is more obvious. However, when TiO 2 With Nb 2 O 5 Ratio of TiO 2 /Nb 2 O 5 When the amount of the glass is more than 0.5, the solar resistance stability of the glass is not improved, but the coloring degree is increased rapidly, and the crystallization resistance is extremely poor, which is contrary to the production objective of obtaining higher transmittance and better crystallization resistance. Therefore, in order to obtain a glass which satisfies the requirements of the optical design and has excellent sunlight resistance stability, tiO 2 /Nb 2 O 5 The value of (2) is 0.5 or less, preferably 0.4 or less, and more preferably 0.2 or less.
For the glass of the system, the ZnO is added into the glass, so that the chemical stability of the glass can be improved, and the high-temperature viscosity of the glass can be reduced, thereby reducing the production difficulty of the glass. However, the inventors have found that if the ZnO content exceeds 7%, the crystallization resistance of the glass rapidly decreases. Therefore, the content of ZnO is limited to 7% or less, preferably 5% or less, and more preferably no ZnO is added.
BaO, caO, srO, mgO all belong to alkaline earth metal oxides, and the refractive index and dispersion of the glass can be adjusted by adding the alkaline earth metal oxides into the glass, so that the stability of the glass is enhanced, and the crystallization resistance of the glass is improved. The general technical literature considers the role of the same oxides in such glasses to be essentially the same. However, the inventors found through many experiments that the above alkaline earth oxides have very different roles for the most important density, chemical stability and crystallization resistance of the glass of the present system.
BaO has the strongest capacity of increasing the density of the glass, so that the content of BaO needs to be limited to be below 15 percent to reach the density expected by the invention; however, if the content is less than 1%, the chemical stability, particularly the water resistance, of the glass is rapidly lowered, and the crystallization resistance of the glass is also rapidly lowered. Therefore, the BaO content is 1 to 15%, preferably 4 to 13%, more preferably 5 to 12%.
SrO has a higher density than CaO but weaker than BaO, and is added to glass to break the chemical stability of the glass, and if the SrO content exceeds 5%, the crystallization resistance of the glass is rather rapidly deteriorated. Therefore, in the present invention, the SrO content is 5% or less, preferably 4% or less, and more preferably 3% or less.
The CaO is added into the glass, so that the refractive index and dispersion of the glass can be improved, the density of the glass is obviously reduced, the glass lens can be light, the high-temperature viscosity and the surface tension of the glass are reduced, and the production difficulty of the glass is reduced. Further, since CaO is the least capable of deteriorating the water resistance among the three alkaline earth metal oxides BaO, caO, srO, it may be added in an appropriate amount from the viewpoint of improving the water resistance of the glass, and in the present invention, the above effect is obtained by adding 23% or less of CaO, preferably the CaO content is 0 to 20%, more preferably 2 to 15%.
For the glass of the system of the invention, if the MgO content exceeds 5%, the crystallization resistance of the glass is rapidly lowered. Therefore, the content of MgO is limited to 5% or less, preferably 3% or less, and more preferably no MgO is added.
It was found through a great deal of experimental study that when BaO, caO, srO alkaline earth oxides are added, the glass undergoes complex synergism, and the performance does not change linearly with the addition of a single substance. When the value of CaO/(BaO+SrO) exceeds 1.0, the chemical stability of the glass is lowered although the density of the glass is lowered to some extent. Therefore, the CaO/(BaO+SrO) value in the present invention is 1.0 or less, preferably 0.01 to 0.9, and more preferably 0.02 to 0.8.
Li 2 O、K 2 O、Na 2 O belongs to alkali metal oxide, and the density of the glass can be reduced by adding an appropriate amount of alkali metal oxide, but the chemical stability and crystallization resistance of the glass can be rapidly reduced. The inventors found through a large number of experimental studies that:
1) In the glass of the system of the present invention, the density of the glass does not decrease linearly with the increase of the alkali metal oxide, but the density does not decrease any more after reaching an extreme value, but the chemical stability of the glass is drastically deteriorated by continuing the addition of the alkali metal oxide to the extreme value. Thus Li 2 O、K 2 O and Na 2 Sum of O contents Li 2 O+K 2 O+Na 2 If the O value exceeds 5%, the glass density is highThe degree is not reduced any more, but the chemical stability is drastically reduced.
From the production point of view, the lower the high-temperature viscosity is, the more favorable the discharge of bubbles is, so that if the density, chemical stability and crystallization resistance of the glass meet the design requirements, not more than 5% of the alkali metal oxide can be added to improve the high-temperature viscosity of the glass and the bubble degree level of the glass. Thus Li 2 O+K 2 O+Na 2 The amount of O is controlled to 5% or less, preferably 4% or less, and more preferably 3% or less.
2) When the above three alkali metal oxides are all present together, a complex synergistic effect is produced if Li 2 O/(K 2 O+Na 2 When the value of O) is more than 0.5, the crystallization resistance and chemical stability of the glass are drastically reduced, and the refractive index temperature coefficient of the glass is substantially unchanged. Thus Li 2 O/(K 2 O+Na 2 O) is 0.5 or less, preferably 0.4 or less, more preferably 0.3 or less, and the density of the glass is reduced, and the crystallization resistance and the chemical stability thereof are reduced little.
From the viewpoint of density reduction, li 2 O and Na 2 O is stronger and K 2 O times; from the viewpoint of breaking the chemical stability of the glass, K 2 O and Na 2 O is stronger and Li 2 O times; in terms of breaking glass crystallization resistance, li 2 The strongest O, K 2 O and Na 2 O times. Therefore, in order to obtain a density, chemical stability and crystallization resistance satisfying the design expectations, a great deal of experimental study is required to determine how to select an appropriate kind and an appropriate amount of alkali metal oxide. If Na is 2 Since the O content exceeds 5%, the crystallization resistance and chemical stability of the glass are drastically reduced, and therefore the content thereof is 0 to 5%, preferably 0.1 to 5%, more preferably 0.5 to 3%. If K 2 The O content is more than 5%, and the crystallization resistance and chemical stability of the glass are rapidly lowered, so that the content thereof is 0 to 5%, preferably 0 to 4%, more preferably 0 to 3%. Li (Li) 2 If the O content exceeds 5%, the crystallization resistance of the glass is rapidly lowered, and Li is therefore 2 The content of O is 0 to 5%, preferably0 to 3%, more preferably no Li is added 2 O。
In some embodiments of the invention, the aggregate value of BaO, srO, caO is equal to La 2 O 3 、Gd 2 O 3 、Y 2 O 3 The ratio of the total value of (2) has a large relationship with the density, crystallization resistance and chemical stability of the glass. When (BaO+SrO+CaO)/(La) 2 O 3 +Gd 2 O 3 +Y 2 O 3 ) When the value of (2) is larger than 2.0, the chemical stability of the glass rapidly decreases; when (BaO+SrO+CaO)/(La) 2 O 3 +Gd 2 O 3 +Y 2 O 3 ) When the glass content is less than 0.4, the chemical stability of the glass is improved, but the density of the glass is rapidly increased, and the crystallization resistance of the glass is rapidly reduced. Therefore, to obtain a glass having a low density, chemical stability meeting design requirements, and good crystallization resistance, it is preferable that (BaO+SrO+CaO)/(La) 2 O 3 +Gd 2 O 3 +Y 2 O 3 ) The value of (2) is 0.4 to 2.0, more preferably 0.5 to 1.8, still more preferably 0.7 to 1.5.
In the glass of the present invention, nb 2 O 5 And La (La) 2 O 3 All are main components, and the ratio has a larger correlation with the refractive index of the glass, the density of the glass and the crystallization resistance. When Nb is 2 O 5 With La 2 O 3 Ratio Nb of (2) 2 O 5 /La 2 O 3 When the glass content is more than 3.0, the density of the glass is not reduced, but the crystallization resistance of the glass is greatly reduced; when Nb is 2 O 5 /La 2 O 3 When the value of (2) is less than 0.8, the refractive index and dispersion of the glass do not meet the design requirements, and the density of the glass rapidly increases. Thus, nb 2 O 5 /La 2 O 3 The value of (2) is 0.8 to 3.0, preferably 1.0 to 2.8, more preferably 1.2 to 2.6.
The inventors have found that in some embodiments of the invention, when (CaO+BaO+SrO)/(Al) 2 O 3 +ZrO 2 +TiO 2 ) When the value of (2) is more than 3.0, although the crystallization resistance of the glass is slightly improved, the refractive index of the glass does not meet the design requirement. Thus, (CaO)+BaO+SrO)/(Al 2 O 3 +ZrO 2 +TiO 2 ) The value of (2) is less than 3.0, preferably less than 2.8, more preferably less than 2.5.
In some embodiments of the invention, the metal is prepared by adding 0 to 1% Sb 2 O 3 、SnO 2 SnO and CeO 2 One or more components of the glass serving as a clarifying agent can improve the clarifying effect of the glass. However, the present invention has a reasonable formulation, and has a good clarifying effect and excellent bubble degree, and therefore, it is preferable to add 0 to 0.5% of the clarifying agent, more preferably 0 to 0.1% of the clarifying agent, and still more preferably, no clarifying agent is added.
< component not to be contained >
In the glass of the present invention, V, cr, mn, fe, co, ni, cu, ag and oxides of transition metals such as Mo are colored even when they are contained in small amounts, either alone or in combination, and absorb at a specific wavelength in the visible light range, so that the property of the present invention of improving the visible light transmittance effect is impaired, and therefore, in particular, an optical glass having a wavelength transmittance in the visible light range is preferably practically not contained.
Th, cd, tl, os, be and Se oxides have a tendency to be used in a controlled manner as harmful chemical substances in recent years, and are required to provide environmental protection not only in the glass manufacturing process but also in the processing steps and disposal after production. Therefore, in the case where the influence on the environment is emphasized, it is preferable that they are not substantially contained except for unavoidable mixing. As a result, the optical glass becomes practically free from environmental pollutants. Therefore, the optical glass of the present invention can be manufactured, processed, and discarded without taking special measures against the environment.
In order to achieve environmental friendliness, the optical glass of the present invention does not contain As 2 O 3 And PbO. Although As 2 O 3 Has the effects of eliminating bubbles and better preventing glass from being colored, but As 2 O 3 The addition of (2) increases the platinum attack of the glass on the furnace, in particular on the platinum furnace, resulting in more platinum ions entering the glass, and thus in a more efficient mannerThe service life of the platinum furnace is adversely affected. PbO can significantly improve the high refractive index and high dispersion properties of glass, but PbO and As 2 O 3 Substances which cause environmental pollution.
The term "not incorporated" as used herein means that the compound, molecule, element or the like is not intentionally added to the optical glass of the present invention as a raw material; however, it is also within the scope of the present invention that certain impurities or components may be present as raw materials and/or equipment for producing optical glass that are not intentionally added, and that may be present in small or trace amounts in the final optical glass.
The performance of the optical glass of the present invention will be described below.
< refractive index and Abbe number >
Refractive index of optical glass (n) d ) With Abbe number (v) d ) Tested according to the method specified in GB/T7962.1-2010.
Refractive index (n) of the optical glass of the present invention d ) 1.82 to 1.90, preferably 1.83 to 1.88, more preferably 1.84 to 1.87; abbe number (v) d ) 27 to 35, preferably 28 to 34, more preferably 28 to 32.
< stability against Water action >
Stability against water action of optical glass (D) W ) (powder method) the test was carried out according to the method specified in GB/T17129.
Stability against water action of the optical glass of the present invention (D W ) The number is 3 or more, preferably 2 or more, and more preferably 1.
< stability against acid action >
Acid action resistance stability of optical glass (D) A ) (powder method) the test was carried out according to the method specified in GB/T17129.
Acid action resistance stability (D) of the optical glass of the present invention A ) The number is 3 or more, preferably 2 or more, and more preferably 1.
< Density >
The density (. Rho.) of the optical glass was measured according to the method prescribed in GB/T7962.20-2010.
The inventionThe density (. Rho.) of the bright optical glass was 4.2g/cm 3 Hereinafter, it is preferably 4.0g/cm 3 Hereinafter, it is more preferably 3.9g/cm 3 Hereinafter, it is more preferably 3.8g/cm 3 The following is given.
< anti-devitrification Property >
Cutting sample glass into 20×20×10mm, and placing at temperature T g Preserving heat for 30 minutes in a muffle furnace at +230 ℃, taking out, putting into heat-preserving cotton, slowly cooling, and observing whether obvious crystallization exists on the surface. The surface no obvious crystallization means that: the surface has no crystallization spots or has crystallization spots, but the area of the crystallization spots accounts for less than 5 percent of the whole area and the crystallization depth is not more than 0.5mm. If the glass sample has no obvious crystallization, the crystallization resistance of the glass is excellent.
< streak degree >
The streak degree of the glass of the present invention was measured according to the method specified in MLL-G-174B. The method is that a fringe instrument consisting of a point light source and a lens is used for comparing and checking the direction of the easiest visible fringe with a standard sample, and the fringe instrument is divided into 4 grades which are A, B, C, D grades respectively, wherein grade A is that no macroscopic fringe exists under the specified detection condition, grade B is that fine and dispersed fringe exists under the specified detection condition, grade C is that no slight parallel fringe exists under the specified detection condition, and grade D is that rough fringe exists under the specified detection condition.
The degree of streaking of the optical glass of the present invention is C or more, preferably B or more, more preferably A.
[ method of production ]
The manufacturing method of the optical glass comprises the following steps: the glass is produced by adopting conventional raw materials and conventional processes, using carbonate, nitrate, sulfate, hydroxide, oxide and the like as raw materials, proportioning according to a conventional method, putting the prepared furnace burden into a smelting furnace at 1300-1350 ℃ for smelting, clarifying, stirring and homogenizing to obtain homogeneous molten glass without bubbles and undissolved substances, and casting and annealing the molten glass in a mould. Those skilled in the art can appropriately select the raw materials, the process methods, and the process parameters according to actual needs.
[ glass preform and optical element ]
The optical glass thus produced may be used to produce a glass preform by using, for example, polishing, reheat press molding, precision press molding, or other press molding means. That is, the glass preform may be produced by mechanically working the optical glass by grinding or polishing, or by producing a preform for press molding from the optical glass, and then performing the polishing after the hot press molding, or by performing the precision press molding on the preform produced by the polishing.
The means for producing the glass preform is not limited to the above-described means. As described above, the optical glass of the present invention is useful for various optical elements and optical designs, and among them, it is particularly preferable to form a preform from the optical glass of the present invention, and use the preform for performing hot press molding, precision press molding, and the like to produce optical elements such as lenses and prisms.
The glass preform and the optical element of the present invention are each formed of the optical glass of the present invention described above. The glass preform of the present invention has excellent characteristics possessed by an optical glass; the optical element of the present invention has excellent characteristics of optical glass, and can provide various optical elements such as lenses and prisms having high optical value.
Examples of the lens include various lenses such as a concave meniscus lens, a convex meniscus lens, a biconvex lens, a biconcave lens, a plano-convex lens, and a plano-concave lens, each of which has a spherical or aspherical lens surface.
[ optical instrument ]
The optical element formed by the optical glass can be used for manufacturing optical instruments such as photographic equipment, vehicle-mounted equipment, camera equipment, display equipment, monitoring equipment and the like.
The optical glass has excellent chemical stability, lower refractive index temperature coefficient and other performances, and is particularly suitable for being applied to the fields of vehicle-mounted, monitoring, security protection and the like.
Examples
< example of optical glass >
In order to further clearly illustrate and describe the technical solutions of the present invention, the following non-limiting examples are provided.
The optical glass shown in tables 2 to 3 was obtained by the above-described method for producing an optical glass. The characteristics of each glass were measured by the test method of the present invention, and the measurement results are shown in tables 2 to 3. In tables 2 to 3, siO 2 /B 2 O 3 The value of (2) is denoted by K1; tiO (titanium dioxide) 2 /Nb 2 O 5 The value of (2) is represented by K2; the value of CaO/(BaO+SrO) is represented by K3; li (Li) 2 O+K 2 O+Na 2 O is represented by K4; (BaO+SrO+CaO)/(La) 2 O 3 +Gd 2 O 3 +Y 2 O 3 ) The value of (2) is denoted by K5; nb (Nb) 2 O 5 /La 2 O 3 The value of (2) is denoted by K6; (CaO+BaO+SrO)/(Al) 2 O 3 +ZrO 2 +TiO 2 ) The value of (2) is denoted by K7; li (Li) 2 O/(K 2 O+Na 2 O) is denoted by K8. In the anti-crystallization performance test, no obvious crystallization is marked as "A", and no obvious crystallization is marked as "B".
TABLE 2
TABLE 3 Table 3
< example of glass preform >
The glasses obtained in examples 1 to 20 were subjected to polishing, hot press molding, and press molding such as precision press molding to prepare preforms of various lenses such as concave meniscus lenses, convex meniscus lenses, biconvex lenses, biconcave lenses, plano-convex lenses, and plano-concave lenses, prisms, and the like.
< example of optical element >
The glass preforms obtained in the above examples were annealed, and fine-tuning was performed while reducing deformation of the inside of the glass, so that optical characteristics such as refractive index reached a desired value.
Next, each preform was ground and polished to produce various lenses and prisms such as a concave meniscus lens, a convex meniscus lens, a biconvex lens, a biconcave lens, a plano-convex lens, and a plano-concave lens. The surface of the obtained optical element may be coated with an antireflection film.
< example of optical instrument >
The optical element manufactured by the above-described optical element embodiments can be used for, for example, imaging devices, sensors, microscopes, medical technology, digital projection, communication, optical communication technology/information transmission, optics/illumination in the automotive field, lithography technology, excimer lasers, wafers, computer chips, and integrated circuits and electronic devices including such circuits and chips, or for imaging devices and apparatuses in the vehicle field, by forming an optical component or an optical assembly by using one or more optical elements through optical design.
Claims (13)
1. The optical glass is characterized by comprising the following components in percentage by weight: siO (SiO) 2 ：3～20％；B 2 O 3 ：8～30％；La 2 O 3 ：8～25％；Nb 2 O 5 : 15-43%; baO:1 to 15 percent of Nb 2 O 5 /La 2 O 3 0.8 to 3.0.
2. The optical glass according to claim 1, further comprising, in weight percent: gd (Gd) 2 O 3 : 0-8%; and/or Y 2 O 3 : 0-5%; and/or Al 2 O 3 :0 to 3 percent; and/or TiO 2 : 0-9%; and/or ZrO 2 : 0-8%; and/or ZnO: 0-7%; and/or MgO: 0-5%; and/or CaO: 0-23%; and/or SrO: 0-5%; and/or Li 2 O: 0-5%; and/or K 2 O: 0-5%; and/or Na 2 O: 0-5%; and/or clarifying agent: 0 to 1 percent.
3. The optical glass is characterized by comprising the following components in percentage by weight 2 ：3～20％；B 2 O 3 ：8～30％；La 2 O 3 ：8～25％；Nb 2 O 5 ：15～43％；BaO：1～15％；Gd 2 O 3 ：0～8％；Y 2 O 3 ：0～5％；Al 2 O 3 ：0～3％；TiO 2 ：0～9％；ZrO 2 ：0～8％；ZnO：0～7％；MgO：0～5％；CaO：0～23％；SrO：0～5％；Li 2 O：0～5％；K 2 O：0～5％；Na 2 O: 0-5%; clarifying agent: 0 to 1%, wherein Nb 2 O 5 /La 2 O 3 0.8 to 3.0.
4. An optical glass comprising SiO 2 、B 2 O 3 、La 2 O 3 、Nb 2 O 5 And an alkaline earth metal oxide, the components of which are expressed in weight percent, wherein SiO 2 /B 2 O 3 0.1 to 1.2, nb 2 O 5 /La 2 O 3 0.8 to 3.0, and the refractive index n of the optical glass d Is 1.82 to 1.90, abbe number v d 27-35, density ρ of 4.2g/cm 3 The following is given.
5. The optical glass according to claim 4, wherein the composition comprises, in weight percent: siO (SiO) 2 : 3-20%; and/or B 2 O 3 : 8-30%; and/or La 2 O 3 : 8-25%; and/or Nb 2 O 5 : 15-43%; and/or BaO: 1-15%; and/or Gd 2 O 3 : 0-8%; and/or Y 2 O 3 : 0-5%; and/or Al 2 O 3 :0 to 3 percent; and/or TiO 2 : 0-9%; and/or ZrO 2 : 0-8%; and/or ZnO: 0-7%; and/or MgO: 0-5%; and/or CaO: 0-23%; and/or SrO: 0-5%; and/or Li 2 O: 0-5%; and/or K 2 O: 0-5%; and/or Na 2 O: 0-5%; and/or clarifying agent: 0 to 1 percent.
6. The optical glass according to any one of claims 1 to 5, wherein the components thereof are expressed in weight percent, wherein: siO (SiO) 2 /B 2 O 3 From 0.1 to 1.2, preferably SiO 2 /B 2 O 3 From 0.12 to 1.0, more preferably SiO 2 /B 2 O 3 From 0.15 to 0.8, siO is more preferable 2 /B 2 O 3 0.15 to 0.3.
7. The optical glass according to any one of claims 1 to 5, wherein the components thereof, expressed in weight percent, satisfy one or more of the following 7 cases:
1)Nb 2 O 5 /La 2 O 3 is 1.0 to 2.8, preferably Nb 2 O 5 /La 2 O 3 Is 1.2 to 2.6, more preferably Nb 2 O 5 /La 2 O 3 1.46 to 2.14;
2)TiO 2 /Nb 2 O 5 is 0.5 or less, preferably TiO 2 /Nb 2 O 5 Is 0.4 or less, more preferably TiO 2 /Nb 2 O 5 At most 0.2, tiO is more preferable 2 /Nb 2 O 5 0.05 to 0.15;
3) CaO/(BaO+SrO) is 1.0 or less, preferably CaO/(BaO+SrO) is 0.01 to 1.0, more preferably CaO/(BaO+SrO) is 0.18 to 1.0, still more preferably CaO/(BaO+SrO) is 0.31 to 0.9, still more preferably CaO/(BaO+SrO) is 0.5 to 0.8;
4)Li 2 O+K 2 O+Na 2 o is 5% or less, preferably Li 2 O+K 2 O+Na 2 O is 4% or less, more preferably Li 2 O+K 2 O+Na 2 O is less than 3%;
5)Li 2 O/(K 2 O+Na 2 o) is 0.5 or less, preferably Li 2 O/(K 2 O+Na 2 O) is 0.4 or less, more preferably Li 2 O/(K 2 O+Na 2 O) is 0.3 or less;
6)(BaO+SrO+CaO)/(La 2 O 3 +Gd 2 O 3 +Y 2 O 3 ) Is preferably (BaO+SrO+CaO)/(La) in the range of 0.4 to 2.0 2 O 3 +Gd 2 O 3 +Y 2 O 3 ) Is 0.5 to 1.8, more preferably (BaO+SrO+CaO)/(La) 2 O 3 +Gd 2 O 3 +Y 2 O 3 ) 0.7 to 1.5;
7)(CaO+BaO+SrO)/(Al 2 O 3 +ZrO 2 +TiO 2 ) The value of (2) is less than 3.0, preferably (CaO+BaO+SrO)/(Al) 2 O 3 +ZrO 2 +TiO 2 ) Is 0.9 to 2.8, more preferably (CaO+BaO+SrO)/(Al) 2 O 3 +ZrO 2 +TiO 2 ) It is more preferably (CaO+BaO+SrO)/(Al) in the range of 1.3 to 2.5 2 O 3 +ZrO 2 +TiO 2 ) 1.48 to 2.2.
8. The optical glass according to any one of claims 1 to 5, wherein the components thereof are expressed in weight percent, wherein: siO (SiO) 2 :3 to 18%, preferably SiO 2 : 4-16%; and/or B 2 O 3 :10 to 28%, preferably B 2 O 3 : 15-25%; and/or La 2 O 3 :10 to 23%, preferably La 2 O 3 : 12-21%; and/or Nb 2 O 5 :20 to 42%, preferably Nb 2 O 5 : 22-40%; and/or BaO: 4-13%, preferably BaO: 5-12%; and/or Gd 2 O 3 :0 to 6%, preferably Gd 2 O 3 :0 to 4 percent; and/or Y 2 O 3 :0 to 3%, preferably Y 2 O 3 :0 to 2 percent; and/or Al 2 O 3 :0 to 2%, preferably Al 2 O 3 :0 to 1 percent; and/or TiO 2 :0.5 to 8%, preferably TiO 2 :1 to 5 percent; and/or ZrO 2 :0.1 to 8%, preferably ZrO 2 : 0.5-7%; and/or ZnO: 0-5%; and/or MgO:0 to 3 percent; and/or CaO:0 to 20%, preferably CaO: 2-15%; and/or SrO:0 to 4%, preferably SrO:0 to 3 percent; and/or Li 2 O:0 to 3 percent; and/or K 2 O:0 to 4%, preferably K 2 O:0 to 3 percent; and/or Na 2 O:0.1 to 5%, preferably Na 2 O:0.5 to 3 percent; and/or clarifying agent: 0 to 0.5%, preferably a clarifying agent: 0 to 0.1 percent.
9. The optical glass according to any one of claims 1 to 5, wherein the optical glass has a refractive index n d 1.82 to 1.90, preferably 1.83 to 1.88, more preferably 1.84 to 1.87; abbe number v d 27 to 35, preferably 28 to 34, more preferably 28 to 32.
10. The optical glass according to any one of claims 1 to 5, wherein the optical glass has a water-action-resistant stability D W Class 3 or more, preferably class 2 or more, more preferably class 1; and/or acid action resistance stability D A Class 3 or more, preferably class 2 or more, more preferably class 1; and/or density ρ of 4.2g/cm 3 Hereinafter, it is preferably 4.0g/cm 3 Hereinafter, it is more preferably 3.9g/cm 3 Hereinafter, it is more preferably 3.8g/cm 3 The following are set forth; and/or the streak degree is C or more, preferably B or more, more preferably a.
11. A glass preform made using the optical glass according to any one of claims 1 to 10.
12. An optical element made using the optical glass according to any one of claims 1 to 10 or made using the glass preform according to claim 11.
13. An optical device comprising the optical glass according to any one of claims 1 to 10, or the optical element according to claim 12.
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| 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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