CN110922053A - Optical glass and optical element - Google Patents

Optical glass and optical element Download PDF

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Publication number
CN110922053A
CN110922053A CN201910885156.5A CN201910885156A CN110922053A CN 110922053 A CN110922053 A CN 110922053A CN 201910885156 A CN201910885156 A CN 201910885156A CN 110922053 A CN110922053 A CN 110922053A
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optical glass
glass
component
optical
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佐佐木勇人
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Hoya Corp
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Hoya Corp
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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
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/23—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron
    • C03C3/247—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron containing fluorine and phosphorus
    • 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
    • C03C4/00—Compositions for glass with special properties
    • 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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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (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)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Glass Compositions (AREA)

Abstract

The invention aims to provide an optical glass with little change of each characteristic of the glass even if the melting time is long. The optical glass of the present invention contains at least F‑And Al3+And F is‑/Al3+Is 3.0 or more, wherein when the optical glass is melted at a given temperature, the amount of change per unit time of nd, vd, Pg, F, D, ng-nF, etc. is extremely low. As the constituent component of the optical glass, O is preferable2‑/(P5++Ti4++Nb5++W6+) Is 3.0 or more.

Description

Optical glass and optical element
Technical Field
The present invention relates to an optical glass and an optical element comprising the optical glass.
Background
Conventionally, in optical glass, pot (pot) melting has been performed in which raw materials are charged into a melting furnace and melted and injected into a mold, but at present, optical glass production by continuous melting that enables continuous production of optical glass has become the mainstream.
The residence time of the continuous melting is constant, and there is no difference in each tank, so that there is an advantage that it is easy to adjust the glass characteristics to be constant.
However, depending on the composition of the glass, the glass characteristics may be easily changed even by continuous melting. For example, when a glass component which is easily volatilized is contained, volatilization proceeds and the composition changes due to a longer melting time, and thus, glass characteristics change.
Particularly, fluorophosphate glass has excellent optical characteristics, but exhibits remarkable volatility in a high-temperature process for melting and molding glass. The volatilization from the melting of the glass during the melting and molding may cause the deterioration of the glass, the variation of the optical characteristics, and the reduction of the uniformity of the glass.
Patent document 1 describes a glass composition for suppressing the fluctuation of glass characteristics, but a technique for suppressing the fluctuation of glass characteristics for a longer time is desired.
Documents of the prior art
Patent document
Patent document 1: japanese laid-open patent publication No. 2007-76958
Disclosure of Invention
Problems to be solved by the invention
Accordingly, an object of the present invention is to provide an optical glass having less variation in each characteristic of the glass even if the melting time is long.
Means for solving the problems
The present inventors have made intensive studies and found the following findings: the present inventors have found that, by setting the composition to a predetermined value, the variation in the characteristic value of the obtained glass due to the melting time is small, and thus the present invention has been completed.
Namely, the present invention is as follows.
[1]An optical glass containing at least F-And Al3+And F is-/Al3+Is 3.0 or more, wherein the absolute value of the amount of change in nd (amount of change per hour) when the optical glass is melted at a given temperature is less than 0.00050.
[2] The optical glass according to [1], wherein,
the optical glass has Pg and F satisfying the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
[3]according to [1]Or [2]]The optical glass contains at least one selected from Ti4+、Nb5+And W6+The component (1).
[4] The optical glass according to any one of [1] to [3],
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
[5]An optical glass containing at least F-And Al3+And F is-/Al3+Is 3.0 or more, wherein the absolute value of the amount of change in vd (amount of change per hour) when the optical glass is melted at a given temperature is less than 1.50.
[6] The optical glass according to [5], wherein,
the optical glass has Pg and F satisfying the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
[7]according to [5]]Or [6]]The optical glass contains at least one selected from Ti4+、Nb5+And W6+The component (1).
[8] The optical glass according to any one of [5] to [7],
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
[9]An optical glass containing at least F-And Al3+And F is-/Al3+Is 3.0 or more, wherein the absolute value of the change amount (change amount per hour) of Pg, F is less than 0.0025 when the optical glass is melted at a given temperature.
[10] The optical glass according to [9], wherein,
the optical glass has Pg and F satisfying the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
[11]according to [9]]Or [10]]The optical glass contains at least one selected from Ti4+、Nb5+And W6+The component (1).
[12] The optical glass according to any one of [9] to [11], wherein,
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
[13]An optical glass containing at least F-And Al3+And F is-/Al3+Is 3.0 or more, wherein the optical glass has a mass change of less than 1.5% from 0 minute to 90 minutes when melted at a given temperature.
[14] The optical glass according to [13], wherein,
the optical glass has Pg and F satisfying the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
[15]according to [13]Or [14]]The optical glass contains at least one selected from Ti4+、Nb5+And W6+The component (1).
[16] The optical glass according to any one of [13] to [15],
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
[17]An optical glass containing at least F-And Al3+And F is-/Al3+Is 3.0 or more, wherein the absolute value of the change amount (change amount per hour) of D (nF-nC) when the optical glass is melted at a given temperature is less than 0.00015.
[18] The optical glass according to [17], wherein,
the optical glass has Pg and F satisfying the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
[19]according to [17]Or [18]]The optical glass contains at least one selected from Ti4+、Nb5+And W6+The component (1).
[20] The optical glass according to any one of [17] to [19],
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
[21]An optical glass containing at least F-And Al3+And F is-/Al3+Is 3.0 or more, wherein the absolute value of the change amount (change amount per hour) of ng-nF is less than 0.00010 when the optical glass is melted at a given temperature.
[22] The optical glass according to [21], wherein,
the optical glass has Pg and F satisfying the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
[23]according to [21]]Or [22]]The optical glass contains at least one selected from Ti4+、Nb5+And W6+The component (1).
[24] The optical glass according to any one of [21] to [23],
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
[25] An optical element comprising the optical glass according to any one of [1] to [24 ].
ADVANTAGEOUS EFFECTS OF INVENTION
The optical glass of the present invention is less likely to cause variations in the properties of the glass due to melting.
Detailed Description
The present invention will be described below, but the present invention is not limited to the specific embodiments.
First, the characteristics of the glass and the composition of the optical glass of the present invention will be described. In the present specification, unless otherwise specified, the content and total content of the cationic component are expressed as cationic% (cation%), and if not specifically specified, the anionic component (in the present specification, O) is contained2-、F-、Cl-、Br-、I-) The content and the total content of (c) are expressed as anion% (anion%).
Here, the cation% is a value calculated as "(number of cations of interest/total number of cations of glass component) × 100", and represents a molar percentage of the amount of cations of interest with respect to the total amount of the cation component.
The anion% is a value calculated as "(number of anions of interest/total number of anions of glass component) × 100", and represents a molar percentage of the amount of anions of interest relative to the total amount of anion components.
The ratio of the contents of the cationic components to each other is equal to the ratio of the contents of the cationic components of interest expressed in cationic%, and the ratio of the contents of the anionic components to each other is equal to the ratio of the contents of the anionic components of interest expressed in anionic%.
The ratio of the content of the cation component to the content of the anion component is calculated as a molar ratio (molar ratio of each atom when the sum of the cation and the anion is 100). For example, for O2-/P5+When the total amount of the cation and the anion is 100, P in the case is used5+Ratio of (A) to (B) and O2-The ratio of (a) to (b) is calculated. In the case of examples, the ratio of the content of the cationic component to the content of the anionic component was calculated in accordance with the ratio shown in Table 2.
The content of the glass constituent component can be determined by a known method, for example, inductively coupled plasma emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS), etc., and in the present invention, the content of the glass constituent component of 0% means that the constituent component is not substantially contained and the content of the constituent component is allowed to be contained at an inevitable impurity level.
The refractive index at each wavelength was measured to the sixth decimal place according to JIS B7071 and expressed as the fifth decimal place. The main dispersions nF-nC (in this specification, nF-nC is sometimes referred to as "D") and ng-nF are also indicated in the decimal five bits. Therefore, the variation of nd, D, ng-nF is expressed in five bits after decimal point.
The abbe number ν d is represented by two digits after a decimal point, and the variation of the abbe number is also represented by two digits after a decimal point.
Pg, F is expressed in four decimal places, and the amount of change in Pg, F is also expressed in four decimal places.
[ optical glass characteristics ]
In the present specification, general values of nd, vd, Pg, F, D, ng-nF of the optical glass are not particularly limited, and are values of 1.5 hours of melting time. When the amount of change per unit time was examined, the amount was calculated from the value obtained when the glass was melted for 2 hours and the value obtained when the glass was melted for 4 hours.
The refractive index nd of the optical glass of the present invention is not particularly limited, and the lower limit thereof may be 1.30000 or more, 1.40000 or more, 1.50000 or more, 1.60000 or more, 1.70000 or more, 1.80000 or more, 1.90000 or more, 2.00000 or more, 2.10000 or more, 2.20000 or more. The upper limit of the refractive index nd may be 2.70000 or less, or 2.60000 or less, 2.50000 or less, 2.40000 or less, 2.30000 or less, 2.20000 or less, 2.10000 or less, 2.00000 or less, 1.90000 or less, 1.80000 or less, 1.70000 or less, 1.60000 or less, 1.50000 or less, or 1.40000 or less.
As one of the characteristics of the optical glass of the present invention, there can be mentioned: the value of nd is not likely to vary regardless of the melting time. Specifically, the absolute value of the amount of change in nd (amount of change per hour) at a given temperature is less than 0.00050. When the amount of change in nd is less than 0.00050, optical glass having nd within a desired range can be obtained even if the melting time varies due to some cause during the production process, and the yield is improved. Preferable upper limits of the absolute value of the amount of change in nd (amount of change per hour) may be, for example, less than 0.00040, less than 0.00030, less than 0.00020, less than 0.00010, less than 0.00005.
The abbe number ν d of the optical glass of the present invention is not particularly limited, and the lower limit thereof may be 10.00 or more, or 15.00 or more, 20.00 or more, 25.00 or more, 30.00 or more, 35.00 or more, 40.00 or more, 45.00 or more, 50.00 or more, 55.00 or more, 60.00 or more, 65.00 or more, 70.00 or more, 75.00 or more, 80.00 or more, 85.00 or more, 90.00 or more, 95.00 or more, or 100.00 or more. The upper limit of the abbe number ν d may be 150.00 or less, or may be 140.00 or less, 130.00 or less, 120.00 or less, 110.00 or less, 100.00 or less, 95.00 or less, 90.00 or less, 85.00 or less, 80.00 or less, 75.00 or less, 70.00 or less, 65.00 or less, 60.00 or less, 55.00 or less, 50.00 or less, 45.00 or less, 40.00 or less, 35.00 or less, 30.00 or less, 25.00 or less, or 20.00 or less.
As one of the characteristics of the optical glass of the present invention, there can be mentioned: the value of vd is not subject to variation regardless of the melting time. Specifically, the absolute value of the amount of change in ν d (amount of change per hour) is less than 1.50. When the variation amount of ν d is less than 1.50, even if the melting time varies due to some cause in the production process, optical glass having ν d within a desired range can be obtained, and the yield is improved. A preferable upper limit of the absolute value of the amount of change (amount of change per hour) of vd may be, for example, less than 1.40, less than 1.30, less than 1.20, less than 1.10, less than 1.00, less than 0.90, less than 0.80, less than 0.70, less than 0.60, less than 0.50, less than 0.40, less than 0.30, less than 0.20, less than 0.10.
The optical glass of the present invention may have an abnormal dispersion property. In the case where the optical glass exhibits positive anomalous dispersion, the optical glass preferably has a composition Pg, F,
Pg,F＞-0.0004νd+0.5718···(1)。
an optical glass satisfying the formula (1) is suitable as an optical glass for correcting a higher-order chromatic aberration. Further, since the composition of an optical glass satisfying the formula (1) is generally rich in volatile components, the yield is improved when the fluctuation of the glass characteristics is small, which is very advantageous in terms of production.
Here, Pg and F are relative partial dispersion and are an index indicating anomalous dispersion. Pg and F are expressed by the following formula (2) using a refractive index nF for an F ray (a wavelength of 486.13nm), a refractive index nC for a C ray (a wavelength of 656.27nm), and a refractive index ng for a g ray (a wavelength of 435.84nm),
Pg,F＝(ng-nF)/(nF-nC)···(2)。
when the optical glass of the present invention has anomalous dispersion, the lower limit of F as Pg may be, for example, 0.5300 or more, 0.5350 or more, 0.5400 or more, 0.5450 or more, and 0.5500 or more.
As one of the characteristics of the optical glass of the present invention, there can be mentioned: the values of Pg and F are not easily changed regardless of the melting time. Specifically, the absolute value of the change amount (change amount per hour) of Pg, F is less than 0.0025. When the absolute value of the amount of change in Pg, F is less than 0.0025, optical glass having Pg, F within a desired range can be obtained even if the melting time varies due to some cause in the production process, and the yield is improved. A preferable upper limit of the absolute value of the amount of change (amount of change per hour) of Pg, F may be, for example, less than 0.0020, less than 0.0015, less than 0.0010, less than 0.0005.
The main dispersion D of the optical glass of the present invention is not particularly limited, and the lower limit thereof may be 0.00400 or more, 0.00450 or more, and 0.00500 or more. The upper limit of D may be 0.01600 or less, or 0.01500 or less, or 0.01400 or less.
As one of the characteristics of the optical glass of the present invention, there can be mentioned: the value of D is not subject to variation regardless of the melting time. Specifically, the absolute value of the change amount (change amount per hour) of D is less than 0.00015. When the amount of change in the absolute value of D is less than 0.00015, optical glass having D within a desired range can be obtained even if the melting time varies due to some cause during the production process, and the yield is improved. Preferable upper limits of the absolute value of the amount of change (amount of change per hour) of D may be, for example, less than 0.00013, less than 0.00010, less than 0.00009, less than 0.00008, less than 0.00007, less than 0.00006, less than 0.00005.
The absolute value of the change amount of D is small, which means that the high-dispersion component does not preferentially volatilize. In addition, main dispersion D has a relationship of (nd-1)/vd.
The ng-nF of the optical glass of the present invention is not particularly limited, and the lower limit thereof may be 0.00100 or more, 0.00150 or more, or 0.00170 or more. The upper limit of ng-nF may be 0.10000 or less, 0.09000 or less, 0.08000 or less.
As one of the characteristics of the optical glass of the present invention, there can be mentioned: the value of ng-nF does not easily vary regardless of the melting time. Specifically, the absolute value of the amount of change (amount of change per hour) of ng-nF is less than 0.00010. When the absolute value of the amount of change in ng-nF is less than 0.00010, optical glass having ng-nF within a desired range can be obtained and yield can be improved even if the melting time varies due to some cause during the production process. The preferable upper limit of the absolute value of the variation (variation per hour) of ng-nF may be, for example, less than 0.00008, less than 0.00007, less than 0.00006, less than 0.00005.
Note that the small absolute value of the amount of change in ng-nF means that the highly dispersed component does not preferentially volatilize.
Further, as one of the characteristics of the optical glass of the present invention, there can be mentioned: the value of the glass quality is not easily changed regardless of the melting time. Specifically, when the melting time of 0 to 90 minutes has elapsed, the absolute value of the amount of change in mass is preferably less than 1.5%. The mass change amounts are, for example, less than 1.4%, less than 1.3%, less than 1.2%, less than 1.1%, and less than 1.0%.
Here, the melting time of 0 minute means that carbonate, nitrate, hydroxide, etc. contained in the batch (batch) raw material (powder raw material of glass) are decomposed, and CO is generated2、NO2、SO3、H2O, etc. in the form of gas.
The optical glass of the present invention is a glass which shows little change in glass properties such as nd, vd, Pg, F, glass quality, D, ng-nF, etc. due to melting, either when the glass is obtained by melting a glass raw material (powder, etc.) or when a material (cullet ) obtained by melting a glass raw material is melted again. That is, the measured values of the properties of the optical glass of the present invention do not easily affect the raw material state of the glass (the state of melting from the powder raw material, the state of melting from the cullet, etc.).
[ optical glass composition ]
The optical glass of the present invention contains at least F-And Al3+And F-And Al3+Molar ratio of (F)-/Al3+) An optical glass having a glass composition of 3.0 or more. From the viewpoint of suppressing the variation in glass properties due to the melting time, F-/Al3+The lower limit of (b) can be set to, for example, 3.1 or more, 3.2 or more, 3.3 or more, 3.4 or more, 3.5 or more, 3.6 or more, 3.7 or more, 3.8 or more, 3.9 or more, or 4.0 or more. In addition, F-/Al3+The upper limit of (b) may be set to, for example, less than 8.0, less than 7.0, less than 6.0.
Hereinafter, the glass component that can be contained in the optical glass of the present invention will be described.
As a component of the optical glass of the present invention, Si4+、P5+And B3+The component (a) is a component constituting the skeleton of the glass and is a component for improving the thermal stability of the glass. Further, the component contributes to a low refractive index and low dispersion. Si4+、P5+And B3+The content of each component is not particularly limited, and may be any content. Si4+、P5+And B3+The upper limit of each component may be, for example, 99% or less, 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less, 20% or less, 15% or less, 10% or less, and 5% or less, respectively, and the lower limit may be, for example, 0% or more, 5% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 60% or more, 70% or more, 80% or more, and 90% or more, respectively.
In addition, for Si4+、P5+And B3+Sum of contents of ingredients (Si)4++P5++B3+) Is not particularly limited, and may take any value, Si4++P5++B3+The upper limit of (b) may be, for example, 99% or less, 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less, 20% or less, 15% or less, 10% or less, or 5% or less. The lower limit may be, for example, 0% or more, 5% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 60% or more, 70% or more, 80% or more, or 90% or more. In addition, Si4+、P5+、B3+Can be used separately or in any combination.
The optical glass of the present invention preferably contains P5+。P5+The component (b) is a component necessary for making the optical glass into a fluorophosphate glass. P5+Component (b) is a readily volatile component, therefore, ifThe effect is very high when the variation in glass properties due to the melting time can be suppressed.
P5+The content is preferably 5 to 50% in terms of cation%.
The optical glass of the present invention contains P5+In the case of component (B), O2-Component (A) and (P)5+Molar ratio of components (O)2-/P5 +) The upper limit of (b) is, for example, 4.4 or less, 4.2 or less, and 4.0 or less, and the lower limit is preferably 2.8 or more and 3.0 or more.
The optical glass of the present invention may contain Li+、Na+、K+、Rb+And Cs+One or more of the components (hereinafter, these components may be referred to as "alkali metal components"). Wherein Li+The component (b) is a component for improving the meltability of the glass, and may improve the thermal stability of the glass. Further, it is a component for lowering the glass transition temperature. Li+、Na+、K+、Rb+And Cs+The content of the component is not particularly limited, and may be any content. As Li+、Na+、K+、Rb+And Cs+The upper limit of each content of the component (b) is, for example, 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less, 20% or less, 15% or less, 10% or less, 7.5% or less, 5.0% or less, 4.0% or less, 3.5% or less, 3.0% or less, 2.5% or less, 2.0% or less, 1.5% or less, 1.0%, 0.5%. The lower limit is, for example, 0% or more, 0.1% or more, 0.5% or more, 1.0% or more, 1.5% or more, 2.0% or more, 2.5% or more, 3.0% or more, 3.5% or more, 4.0% or more, 5.0% or more, 7.5% or more, 10.0% or more, 15.0% or more, 20.0% or more, 25.0% or more, 30.0% or more, 35.0% or more, 40.0% or more, 45.0% or more, 50.0% or more, 60.0% or more, 70.0% or more, or 80.0% or more.
Mg2+、Ca2+、Sr2+、Ba2+And Zn2+Component (b) is a component for improving the meltability of glass, and may improve the glassThermal stability of (2). In addition, Mg2+、Ca2+、Sr2+、Ba2+And Zn2+The component (A) is a component which lowers the glass transition temperature, and Li+、Na+、K+、Rb+And Cs+The composition may sometimes increase the refractive index. For Mg2+、Ca2+、Sr2+、Ba2+And Zn2+The respective contents of the components are also not particularly limited. Mg (magnesium)2+、Ca2+、Sr2+、Ba2+And Zn2+The upper limit of the content of each component may be 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less, 20% or less, 15% or less, 10% or less, 7% or less, 5% or less, 3% or less, 1% or less, or 0.5% or less.
Mg2+、Ca2+、Sr2+、Ba2+And Zn2+The lower limit of the content of each component may be, for example, 0% or more, 1% or more, 3% or more, 5% or more, 7% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 60% or more, 70% or more, 80% or more, or 90% or more.
For Mg2+、Ca2+、Sr2+、Ba2+And Zn2+Sum of respective contents of ingredients (Mg)2++Ca2++Sr2++Ba2++Zn2+) Also not particularly limited, Mg2++Ca2++Sr2++Ba2++Zn2+The upper limit of (b) may be, for example, 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less, 20% or less, 15% or less, 10% or less, 7% or less, 5% or less, 3% or less, 1% or less, or 0.5% or less.
Mg2+、Ca2+、Sr2+、Ba2+And Zn2+Sum of respective contents of ingredients (Mg)2++Ca2++Sr2++Ba2++Zn2+) The lower limit of (b) may be, for example, 0% or more, 1% or more, 3% or more, 5% or more, 7% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 60% or more, 70% or more, 80% or more, or 90% or more.
La3+、Gd3+、Y3+And Yb3+The component (B) is a compound of with Mg2+、Ca2+、Sr2+、Ba2+The component having a higher refractive index than the component having a higher refractive index is a component contributing to a higher refractive index and a lower dispersion. May also be obtained by introducing La3+、Gd3+、Y3+And Yb3+The components improve the thermal stability of the glass. La3+、Gd3+、Y3+And Yb3+The respective contents of the components are not particularly limited, and La3+、Gd3+、Y3+And Yb3+The upper limit of the content of each component may be, for example, 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less, 20% or less, 15% or less, 10% or less, 7% or less, 5% or less, 3% or less, 1% or less, or 0.5% or less.
La3+、Gd3+、Y3+And Yb3+The lower limit of the content of each component may be, for example, 0% or more, 1% or more, 3% or more, 5% or more, 7% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 60% or more, 70% or more, or 80% or more.
La3+、Gd3+、Y3+And Yb3+Sum of contents of ingredients (La)3++Gd3++Y3++Yb3+) Also, La is not particularly limited3++Gd3++Y3++Yb3+The upper limit of (B) may be 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less, 20% or less, 15% or less, 10% or less, 7% or less, 5% or less, or more,Less than 3%, less than 1%, less than 0.5%.
La3++Gd3++Y3++Yb3+Sum of contents of ingredients (La)3++Gd3++Y3++Yb3+) The lower limit of (b) may be 0% or more, 1% or more, 3% or more, 5% or more, 7% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 60% or more, 70% or more, 80% or more, or 90% or more.
Ti4+、Nb5+、Ta5+、W6+And Bi3+The component contributes to a high refractive index and high dispersion, and may improve the thermal stability of the glass as a network-forming component. Ti4+、Nb5+、Ta5+、W6+And Bi3+The respective contents of the components are not particularly limited, and Ti4+、Nb5+、Ta5+、W6+And Bi3+The upper limit of the content of each component may be 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less, 20% or less, 15% or less, 10% or less, 7% or less, 5% or less, 3% or less, 1% or less, or 0.5% or less.
Ti4+、Nb5+、Ta5+、W6+And Bi3+The lower limit of each content of the component (a) may be 0% or more, 1% or more, 3% or more, 5% or more, 7% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 60% or more, 70% or more, or 80% or more.
Ti4+、Nb5+、Ta5+、W6+And Bi3+Sum of respective contents of components (Ti)4++Nb5++Ta5++W6++Bi3+) Also, the content is not particularly limited, and may be, for example, 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less,20% or less, 15% or less, 10% or less, 7% or less, 5% or less, 3% or less, 1% or less, 0.5% or less.
Ti4+、Nb5+、Ta5+、W6+And Bi3+Sum of respective contents of components (Ti)4++Nb5++Ta5++W6++Bi3+) The lower limit of (b) may be, for example, 0% or more, 1% or more, 3% or more, 5% or more, 7% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 60% or more, 70% or more, or 80% or more.
The optical glass of the present invention preferably contains at least one element selected from Ti4+、Nb5+、W6+The component (1). In the case of an optical glass having an abnormal dispersibility, Ti may be added4+、Nb5+、W6+To increase Pg, F. Addition of these components is preferable because Pg and F higher than those of the above formula (1) can be obtained in some cases.
The optical glass of the present invention contains P5+Component (A) and Ti4+In the case of component (b), O is a compound that suppresses volatilization of the component in a molten state of the glass2-Component (A) and (P)5+Component + Ti4+Molar ratio of components (O)2-/(P5++Ti4+) The lower limit of) is preferably 2.8 or more and 3.0 or more. The upper limit is preferably 4.0 or less, 3.8 or less, 3.6 or less, and 3.4 or less, for example.
The optical glass of the present invention contains P5+Component (B) and Nb5+In the case of component (b), O is a compound that suppresses volatilization of the component in a molten state of the glass2-Component (A) and (P)5+Component + Nb5+Molar ratio of components (O)2-/(P5++Nb5+) The lower limit of) is preferably 2.8 or more and 3.0 or more. The upper limit is preferably 4.0 or less, 3.8 or less, 3.6 or less, and 3.4 or less, for example.
The optical glass of the present invention contains P5+Component (A) and W6+In the case of component (b), O is a compound that suppresses volatilization of the component in a molten state of the glass2-Component (A) and (P)5+Component + W6+Molar ratio of components (O)2-/(P5++W6+) The lower limit of) is preferably 2.8 or more and 3.0 or more. The upper limit is preferably 4.0 or less, 3.8 or less, 3.6 or less, or 3.4 or less, for example. W6+The addition of (3) is effective for Pg, but if contained in excess, there is a risk that the specific gravity becomes too large.
As described above, provided that O is present2-/(P5++Ti4+)、O2-/(P5++Nb5+) And O2-/(P5++W6+) When the amount is a predetermined value or more, volatilization of components can be suppressed in a molten state of the glass. It is considered that this is due to Ti4+、Nb5+、W6+Such cations readily enter the phosphate network.
Therefore, from the viewpoint of volatilization of the components, O is2-Component to P5+、Ti4+、Nb5+、W6+The total amount of (c) is preferably a given ratio or more. Specifically, O2-/(P5++Ti4++Nb5++W6+) Preferably 3.0 or more. O is2-/(P5++Ti4++Nb5++W6+) When the amount is 3.0 or more, it is preferable to reduce volatilization from the glass melt. O is2-/(P5++Ti4++Nb5++W6+) More preferably 3.1 or more, still more preferably 3.15 or more, and particularly preferably 3.2 or more. In addition, O2-/(P5++Ti4++Nb5++W6+) Preferably 4.0 or less, more preferably 3.8 or less, further preferably 3.6 or less, and further preferably 3.4 or less.
Zr4+And Al3+Component (b) is a component for improving chemical durability, sometimes by introducing Zr4+、Al3+Ingredients, which improve the thermal stability of the glass. In addition, Al3+And also has an effect of improving processability. Zr4+And Al3+The respective contents of the components are also not particularly limited, Zr4+And Al3+The upper limit of the content of each component may be, for example, 60% or less, 50% or less, 40% or less, 35% or less, 30% or less, 20% or less, 15% or less, 10% or less, 9% or less, 8% or less, 7%, 6% or less, 5% or less, 4% or less, 3% or less, 2% or less, 1% or less, or 0.5% or less.
Zr4+And Al3+The lower limit of the content of each component may be, for example, 0% or more, 1% or more, 3% or more, 4% or more, 5% or more, 6% or more, 7% or more, 8% or more, 9% or more, 10% or more, 15% or more, 20% or more, 30% or more, 35% or more, 40% or more, or 50% or more.
In particular, Al3+The optical glass of the present invention is an important component, and in the above range, the cation% is preferably 5 to 50%.
The technique for suppressing the variation of the optical characteristics of the present invention can be applied to all optical glasses, particularly those containing P5+、Al3+、O2-、F-The optical glass of (2) can be easily confirmed for its properties.
Note that, regarding P5+With Al3+Is not particularly limited, whether it is for P5+Optical glass, or Al3+The effect was confirmed with a relatively large amount of glass.
At least one kind of cation selected from As, Sb and Sn may be added to the glass As required. Cations of As, Sb and Sn have a clarifying effect during melting of the glass and an effect of reducing bulk platinum in the obtained glass. In addition, the oxidation/reduction state of the glass may be adjusted. The content of the cation of As, Sb, and Sn is not particularly limited, and the upper limit of the content of the cation of As, Sb, and Sn may be 1% or less, 0.9% or less, 0.8% or less, 0.7% or less, 0.6% or less, 0.5% or less, 0.4% or less, 0.3% or less, 0.2% or less, 0.1% or less, 0.09% or less, 0.08% or less, 0.07% or less, 0.06% or less, 0.05% or less, 0.04% or less, 0.03% or less, 0.02% or less, 0.01% or less, 0.009% or less, 0.008% or less, 0.007% or less, 0.006% or less, 0.004% or less, 0.003% or less, 0.002% or less, and 0.001% or less. The lower limit of the content of each of the As, Sb, and Sn cations may be 0% or more, 0.001% or more, 0.002% or more, 0.003% or more, 0.004% or more, 0.005% or more, 0.006% or more, 0.007% or more, 0.008% or more, 0.009% or more, 0.01% or more, 0.02% or more, 0.03% or more, 0.04% or more, 0.05% or more, 0.06% or more, 0.07% or more, 0.08% or more, 0.09% or more, 0.1% or more, 0.2% or more, 0.3% or more, 0.4% or more, 0.5% or more, 0.6% or more, 0.7% or more, 0.8% or more, and 0.9% or more.
O of the invention2-Has the function of keeping the thermal stability of the glass. O is2-The upper limit of the content may be 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less, 20% or less, 15% or less, 10% or less, 7% or less, 5% or less, 3% or less, 1% or less, or 0.5% or less with respect to the total amount of the anionic component.
O2-The lower limit of the content may be, for example, 0% or more, 1% or more, 3% or more, 5% or more, 7% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 60% or more, 70% or more, or 80% or more with respect to the total amount of the anionic component.
In a system in which the following halide ions are not introduced, O2-Typically 100%. On the other hand, in the case of the fluorophosphoric acid-based glass, for example, it can be set to 10 to 80% in terms of anion%.
F as an anionic component may be added to the optical glass of the present invention-、Cl-、Br-、I-And (4) plasma halide ions. F-、Cl-、Br-、I-The upper limit of the content may be 90% or less, 80% or less, 70% or less, 60% or less, 50% or less, 45% or less, 40% or less, 35% or less, 30% or less, 25% or less, 20% or less, 15% or less, respectivelyLower, 10% or less, 7% or less, 5% or less, 3% or less, 1% or less, 0.5% or less.
F-、Cl-、Br-、I-The lower limit of the content of each component may be, for example, 0% or more, 1% or more, 3% or more, 5% or more, 7% or more, 10% or more, 15% or more, 20% or more, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 60% or more, 70% or more, or 80% or more with respect to the total amount of the anionic component.
Particularly, F as an important component in the present invention-Preferably, the anion% is 20 to 90%.
Among these, F is introduced-And Cl-The dispersion can be reduced, and the glass has an effect of imparting abnormal dispersibility to the glass, an effect of lowering the glass transition temperature, and an effect of improving chemical durability.
When it is a problem that a radioactive substance is contained in a material depending on the application, it is preferable that the content of the radioactive isotope is suppressed to a certain amount or less, or the radioactive isotope is intentionally not contained (but the incorporation as an impurity is not prevented).
[ method for producing optical glass ]
The optical glass of the present invention can be obtained by, for example, blending, melting, and molding glass raw materials so as to obtain predetermined characteristics. As the glass raw material, for example, phosphate, fluoride, alkali metal compound, and alkaline earth metal compound may be used. The melting method and the molding method of glass may be any known methods.
It should be noted that the "given temperature" for melting in the present invention means a temperature at which the glass can be completely melted. The specific given temperature is (A)950 ℃ or (B) a temperature at which melting occurs at the liquidus temperature of the glass (hereinafter sometimes referred to as LT) +150 ℃ to 400 ℃ (LT plus 150 ℃ to LT plus 400 ℃). Therefore, the given temperature satisfies either of the above (a) or (B). The specific predetermined temperature is 650 ℃, 700 ℃ or higher, 750 ℃ or higher, 800 ℃ or higher, 850 ℃ or higher, 900 ℃ or higher as the lower limit, and is, for example, 1500 ℃ or lower, 1450 ℃ or lower, 1400 ℃, 1350 ℃, 1300 ℃, 1250 ℃, 1200 ℃, 1150 ℃, 1100 ℃, 1050 ℃, 1000 ℃, 950 ℃. For example, when the optical glass of the present invention is a fluorophosphate glass, examples of the "predetermined temperature" include: 850. 900 deg.C, 950 deg.C, 1000 deg.C, 1050 deg.C, 1100 deg.C, 1150 deg.C.
In the present specification, LT at the time of determining a given temperature may be determined as described below.
(1) First, a platinum crucible was charged with cullet of a given composition having a volume of 12.5 ml. + -. 2.0ml in N2The mixture was kept in a gas atmosphere at a temperature sufficient for melting for 2 hours. The glass was observed after 2 hours of holding, and no crystal deposition was observed.
(2) The temperature was lowered by 50 ℃ and the same experiment was carried out, and the lowest temperature at which no crystal deposition was observed was defined as LT. For example, when the crystal is "present" at 800 ℃, the crystal is "absent" at 850 ℃ and the crystal is "absent" at 900 ℃, LT is represented at 850 ℃.
The presence or absence of crystal precipitation was judged by whether or not crystals were observed at the interface between the glass and the platinum crucible and in the glass by an optical microscope. When crystals having a crystal size of 10 μm or more were observed, it was judged that "crystals were present".
For example, a platinum crucible having a bottom inner diameter of 30mm to 60mm may be used. The platinum crucible may be in the shape of a cylinder, a truncated cone, or the like.
It is preferable that the molten glass obtained by melting cullet is cooled for each platinum crucible and observed with an optical microscope without taking out a sample from the crucible. Therefore, the thickness of the glass sample is preferably 1 to 10mm, more preferably 2 to 5mm at room temperature.
The atmosphere of the optical glass of the present invention during melting can be appropriately changed depending on the material of the optical glass. For example, if it is Si4+Glass containing B as main component3+And La3+Glass containing as main component B3+、La3+、Nb5+The glass as the main component may be in the atmosphere, a non-oxidizing gas atmosphere, a reducing gas atmosphere, or the like, or in the case of a fluorophosphate glass, it may be in a non-oxidizing gas atmosphere (specifically, N)2Gas atmosphere, Ar gas atmosphere, etc.) and the like.
Examples
The present invention will be described in detail below with reference to examples, but the present invention is not limited to the examples.
(measurement of optical glass Properties)
Raw materials such as optical glass grade high purity oxides, hydroxides, carbonates, nitrates, chlorides, fluorides, sulfates and the like were weighed and mixed to obtain glasses having compositions of examples/comparative examples in table 1, to obtain formulated raw materials. Next, each prepared raw material was placed in a platinum crucible, heated to a predetermined temperature as described above, melted in a nitrogen atmosphere for 2 hours or 4 hours from the start of melting, stirred and homogenized, and then allowed to stand, clarified, and then poured into a mold. After the glass solidified, the glass was moved to an electric furnace previously heated to the vicinity of the annealing point of the glass, and gradually cooled to room temperature. Thus, glass-formed blocks of examples/comparative examples were produced. Test pieces necessary for measurement were cut out from each of the obtained glass blocks, and subjected to polishing processing to evaluate the properties. The results of the changes in the respective characteristics are shown in table 4.
(1) Determination of nd, ng, nF, nC and Abbe number vd
The glass obtained by cooling at a cooling rate of-30 ℃/hr was subjected to the measurement of refractive index nd, ng, nF, nC and Abbe number ν d by the refractive index measurement method of JIS B7071.
(2) Determination of relative partial Dispersion Pg, F
The relative partial dispersions Pg, F were calculated from nd, ng, nF, and nC obtained in (1) above.
(measurement of glass Mass Change)
As a glass batch, a batch raw material of glass was prepared so that the yield a reached 150 to 200g, the batch raw material was put into a platinum crucible, a platinum lid was covered, and the mass of the batch raw material, the platinum crucible, and the lid was measured. Then, the platinum crucibles in which the batch materials were placed were covered, and the batch materials of each crucible were placed in a glass melting furnace and heated at 900 ℃, 950 ℃, 1050 ℃, or 1100 ℃ for 1.5 hours (90 minutes) to melt the glass. After 1.5 hours (90 minutes) had elapsed, the mass of the platinum crucible was measured for each content (molten glass) in a state where a platinum cap was covered.
When the total mass of the platinum crucible, the platinum cap, and the batch raw material before melting the glass is denoted by B, the mass of the batch raw material is denoted by C, and the total mass of the platinum crucible, the platinum cap, and the molten glass after melting the glass is denoted by D, the mass of the glass component lost from the molten glass in the crucible due to volatilization during melting is denoted by { B- (C-A) } -D. C-A is the mass of gas generated by thermal decomposition of the batch materials upon heating. The gas is not a glass component, but is, for example, CO generated when carbonates, nitrates, sulfates, hydroxides, etc. are used in the batch raw materials and they are thermally decomposed2、NO2、SO3、H2O, and the like. The amount of these gases generated can be calculated by a known method. In the present specification, B- (C-A) is defined as the glass mass at a melting time of 0 hour.
The amount of volatilization of the glass component before and after melting is determined as a value obtained by dividing the mass ({ B- (C-A) } -D) of the glass component lost from the molten glass in the crucible by volatilization during melting by the glass yield, i.e., [ { B- (C-A) } -D ]/A percentage. The results of the change in glass quality are shown in Table 3.
The compositions of glasses used in examples and comparative examples are shown in table 1 (cation% and anion%) and table 2 (element ratio). The glass properties that are the references for each glass are shown in table 3. The values nd, vd, Pg, F, D, ng-nF in Table 3 are values obtained when the glass was melted for 1.5 hours.
The LT in table 3 is a value measured by the method described in the specification. The glass used in the measurement was 50g, and the volume of the glass was within a range of 12.5 ml. + -. 2.0 ml.
Figure BDA0002207090030000171
Figure BDA0002207090030000181
Figure BDA0002207090030000191
Figure BDA0002207090030000201
According to the examples and comparative examples, Al is added3+/F-In the given range, even when the melting time is increased from 2 hours to 4 hours (from 0 minute to 90 minutes with respect to the glass quality), the variation in glass characteristics such as nd, vd, Pg, F, glass quality, D, ng-nF is extremely small.
The optical glass of the present invention can be used as a material for optical elements.

Claims (25)

1. An optical glass containing at least F-And Al3+And F is-/Al3+The content of the organic acid is more than 3.0,
wherein the absolute value of the amount of change in nd thereof when the optical glass is melted at a given temperature is less than 0.00050, the amount of change being the amount of change per hour.
2. The optical glass according to claim 1,
pg, F of the optical glass satisfies the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
3. the optical glass according to claim 1 or 2, which contains at least one element selected from Ti4+、Nb5+And W6+The component (1).
4. The optical glass according to any one of claims 1 to 3,
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
5. An optical glass containing at least F-And Al3+And F is-/Al3+The content of the organic acid is more than 3.0,
the optical glass has an absolute value of the amount of change in vd, which is the amount of change per hour, of less than 1.50 when melted at a given temperature.
6. The optical glass according to claim 5,
pg, F of the optical glass satisfies the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
7. the optical glass according to claim 5 or 6, which contains at least one element selected from Ti4+、Nb5+And W6+The component (1).
8. The optical glass according to any one of claims 5 to 7,
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
9. An optical glass containing at least F-And Al3+And F is-/Al3+The content of the organic acid is more than 3.0,
wherein the optical glass has an absolute value of a change amount of Pg, F, which is a change amount per hour, of less than 0.0025 when melted at a given temperature.
10. The optical glass according to claim 9,
pg, F of the optical glass satisfies the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
11. the optical glass according to claim 9 or 10, which contains at least one element selected from the group consisting of Ti4+、Nb5+And W6+The component (1).
12. The optical glass according to any one of claims 9 to 11,
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
13. An optical glass containing at least F-And Al3+And F is-/Al3+The content of the organic acid is more than 3.0,
wherein the optical glass has a mass change of less than 1.5% from 0 minute to 90 minutes when melted at a given temperature.
14. The optical glass according to claim 13,
pg, F of the optical glass satisfies the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
15. the optical glass according to claim 13 or 14, which contains at least one element selected from Ti4+、Nb5+And W6+The component (1).
16. The optical glass according to any one of claims 13 to 15,
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
17. An optical glass containing at least F-And Al3+And F is-/Al3+The content of the organic acid is more than 3.0,
wherein the optical glass has an absolute value of a change amount of D (nF-nC) of less than 0.00015 when melted at a given temperature, the change amount being a change amount per hour.
18. The optical glass according to claim 17,
pg, F of the optical glass satisfies the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
19. the optical glass according to claim 17 or 18, which contains at least one element selected from Ti4+、Nb5+And W6+The component (1).
20. The optical glass according to any one of claims 17 to 19,
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
21. An optical glass containing at least F-And Al3+And F is-/Al3+The content of the organic acid is more than 3.0,
wherein the optical glass has an absolute value of a variation in ng-nF, which is a variation per hour, of less than 0.00010 when melted at a given temperature.
22. The optical glass of claim 21, wherein,
pg, F of the optical glass satisfies the following formula (1):
Pg,F＞-0.0004νd+0.5718···(1)。
23. the optical glass according to claim 21 or 22, which contains at least one element selected from Ti4+、Nb5+And W6+The component (1).
24. The optical glass according to any one of claims 21 to 23,
O2-/(P5++Ti4++Nb5++W6+) Is 3.0 or more.
25. An optical element comprising the optical glass as defined in any one of claims 1 to 24.
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