CN1216822C - Lead-free optical barium flint glass - Google Patents

Lead-free optical barium flint glass Download PDF

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Publication number
CN1216822C
CN1216822C CN 98119951 CN98119951A CN1216822C CN 1216822 C CN1216822 C CN 1216822C CN 98119951 CN98119951 CN 98119951 CN 98119951 A CN98119951 A CN 98119951A CN 1216822 C CN1216822 C CN 1216822C
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Prior art keywords
glass
weight
flint glass
barium flint
tio
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CN1214324A (en
Inventor
U·科尔贝里
A·维特泽尔
M·温克勒尔－特鲁德维格
M·吉尔克
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Schott AG
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Schott Glaswerke AG
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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
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
    • 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
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

To profitably produce a lead-free optical barium flint glass having good meltability and processability, very high chemical resistance, a refractive index nd of 1.55-1.66 and an Abbes's number &eta d of 39-52. SOLUTION: The glass is a compsn. consisting of, by weight on the oxide basis, 40-60% SiO2 , 6.5-12% B2 O3 , 10-35% BaO, 0-1% CaO, 0-2% ZnO, 5-12% TiO2 , 0.5-3.5% Al2 O3 , 3-7.5% Na2 O and 3-8% K2 O (Na2 O+K2 O <=15%) and optionally contg. a usual amt. of a refining agent. The glass exhibits positive abnormal or normal partial dispersion in the blue region of its spectrum.

Description

Lead-free optical barium flint glass
The present invention relates to a kind of refractive index n dBe 1.55-1.66 and abbe number V dNo aluminium optical barium flint glass for 39-52.
Different with the classification of common industrial glass is (having abbe number according to this classification barium flint glass is 43-50), and the term barium flint glass also comprises and is up to the higher or lower Abb of above-mentioned ultimate in this application.
Because generally proposed some problems in recent years, as glass component PbO and As 2O 3To environment safety whether, some opticinstrument manufacturerss are just turning to and are only using no PbO and no As 2O 3Glass.Therefore the such glass that has corresponding optical property should be able to have been bought on market.
In producing the foam glass component, that is to say that low density glass also wishes to eliminate PbO.
Usually, it is impossible only replacing plumbous oxide to produce being subjected to the desirable optics that PbO influences and the glass of mechanical property with one or more components.On the contrary, need a kind of new glass composition of development, or make them make a large amount of variations at least.
Patent documentation has comprised a large amount of data, has wherein described its optical value in these scopes and near the crown glass of described scope.Yet these glass have a large amount of shortcomings.For example, JP60-221338A has described the glass that has high relatively specific refractory power sometimes, and it must contain Y 2O 3, La 2O 3, B 2O 3And Li 2O, SiO simultaneously 2It only is a kind of selection component.Because Y 2O and La 2O 3Content can reach 20% weight respectively or reach 52% weight, so for method for continuous production, this glass is expensive with uneconomic.Because very high sometimes B 2O 3Content (reaching 50% weight) and have Li 2O, the poor chemical stability of this glass, the two makes them be difficult to further handle and limited its use.Li 2O has reduced the crystal stability of glass.In addition, the glass of describing in JP3-5341A that has quite high abbe number sometimes needs Li 2O and relative high La 2O 3Content.
In addition, the glass in patent US2433883 and US2523266 must contain Li 2O.They also contain ZrO 2(being respectively 4-15% weight and 2-15% weight), this makes the easier crystallization of glass.As for the ZrO that in US2523265, has 6-8% weight 2Glass, the back one viewpoint also be proved.
For Nb 2O 5, it exists and La 2O 3And Y 2O 3Similar problem.These oxide compounds have increased total price, so production cost is huge.In the glass described in patent DE1496524 and JP6-107425A and the JP52-45612A, it is a neccessary composition.Preceding a kind of glass has very high specific refractory power (at least 1.65).In back two kinds of glass, need Nb 2O 5Alleviate the influence of very high sometimes alkali metal oxide content (reaching 30% weight and 40% weight respectively) to chemical stability and crystallization-stable extreme difference.
The glass that proposes among alumina-free glass among the SU975617 and the JP5-17176A needs SrO.They contain quantity respectively is this component that is no more than 20% weight and is no more than 14% weight.Contain ZrO among the US5300467 2Glass also contain the SrO that is no more than 20% weight.Because SrO is similar to the effect of BaO and CaO to the effect of optical property, then a component can be incorporated in the glass by quite cheap raw material, if can save SrO, helps economic production.
Glass with high BaO content has been described, wherein TiO among the JP56-73646A 2Only be a kind of optional component, 3% weight at the most.At least when no PbO, these glass can not reach the optical states of high refractive index and low abbe number.And their chemical stability is bad.
The concentration of aluminum oxide is very high in the glass of JP1-133956A.If particularly unique optional component B 2O 3When not existing, this makes glass be difficult to fusing.
Do not contain or only contain small amounts of alkali metal oxides in the glass among the DE-B1918350.The relatively poor meltability that causes therefrom remedies by the fluorine of 2%-14.5% weight.Because these high fluorine content in large-scale production, purify and contain HF and SiF 4Waste gas be the difficulty and the costliness.
The purpose of this invention is to provide a kind of refractive index n dBe 1.55-1.66 and abbe number V dBe the unleaded barium flint glass of 39-52, but this glass has good fusing and processing characteristics, can economic production and have very high chemical stability.Back one characteristic is important to further processing and its application possibility of glass.
This purpose can reach by glass of the present invention.
The glass that this glass contains 40-60% weight forms compound S iO 2When lower content, will reduce the acid resistance of glass, and when higher content, will damage its meltability.
In order to improve acid resistance, this glass contains the aluminum oxide of at least 0.5% weight and the TiO of at least 5% weight 2Yet, the maximum level of these oxide compounds of should exceed not, the TiO of aluminum oxide of 3.5% weight (preferred 3% weight) and 12% weight 2, otherwise will damage its meltability again.TiO 2Not only improve chemical stability, and reach high specific refractory power, and particularly when high specific refractory power, be used to finely tune abbe number.
In preferred version of the present invention, because they are to the double effects of acid resistance and meltability, regulation is with said oxide compound (SiO 2+ Al 2O 3+ TiO 2) total amount be restricted to the 47-72% total amount.
Glass contains the Na of 3-7.5% weight 2The K of O and 3-8% weight 2O stipulates Na simultaneously 2O and K 2The total amount of O is should exceed 15% total amount not.These alkalimetal oxides are used to improve meltability.When lower content, temperature of fusion can not reduce fully, and therefore economic production becomes more difficult.When higher content, thermal expansivity increases, and has reduced transition temperature and has damaged chemical stability.
This glass also contains the B of 6.5-12% total amount 2O 3Because this component, meltability improves equally, and in this case, does not need to consider the expansible negative effect.Yet, when extremely high content, reduced chemical stability, particularly alkali resistance.Preferably maximum level is restricted to 11% weight.
According to the content of the oxide compound that occurs in denominator, what represent the particularly preferred concrete scheme of the present invention is with B 2O 3/ (SiO 2+ TiO 2+ Al 2O 3) thereby ratio is restricted at the most 0.20 to B 2O 3Content limit.Those glass that reach this condition have extraordinary alkali resistance.Along with the increase of this ratio, this alkali resistance just reduces, to such an extent as to when 0.2 value is above, no longer can reach best alkali resistance grade, 1 grade.
In order to reach desirable abbe number scope, glass contains the BaO of 10-35% weight.When lower content, can not reach abbe number, and when higher content, the susceptibility of devitrification increases in the barium flint glass scope.In order to improve crystallization-stable, glass can contain the CaO that is no more than 1% weight and be no more than the ZnO of 2% weight.The CaO and/or the ZnO of preferred at least 0.1% weight are in particular the CaO of at least 0.1% weight.If surpass the CaO and the ZnO of aforementioned maximum level, it will be more difficult reaching high specific refractory power and high abbe number so.
Existing in the application's applicant company (official's files are with reference to P19703391.1) still openly in German application during day, a kind of lead-free optic glass has been described, it is overlapping aspect specific refractory power and abbe number with the glass of describing in this application, and has similar composition.Compare with these glass, here can save fully in the glass of Miao Shuing and use ZrO 2, this is owing to do not have ZrO in this glass 2So they can melt under lower temperature, and can produce more economically.Because higher Na 2O content, this glass has meltability preferably.
In the desired compositing range of the independent claim of glass, two kinds of preferred compositing ranges are arranged with aforementioned specific refractory power and abbe number.A kind of glass that makes has high specific refractory power, and another kind makes glass have low specific refractory power:
Have high BaO content and low-down SiO 2The glass of content has following composition (is the weight % of benchmark with the oxide compound):
SiO 241-48; B 2O 36.5-8; BaO 28-35; CaO 0.5-1; ZnO 1-2; TiO 25-12; Al 2O 30.5-1.5; Na 2O 3-5; K 2O 3-5; Na wherein 2O+K 2O 6.5-8;
The refractive index n of these glass dBe 1.60-1.66 and abbe number v dBe 39-52.
What have low BaO content is rich in SiO relatively 2Glass have following composition (is the weight % of benchmark with the oxide compound):
SiO 246-59; B 2O 36.5-8.5; BaO 10-28 (preferred 10-＜28); CaO 0.1-1; ZnO0-2; TiO 2(6.5-12 preferred 7-12); Al 2O 30.5-2; Na 2O 3-7.5; K 2O 3-7.5;
Na wherein 2O+K 2O 〉=6.5;
The refractive index n of these glass dBe 1.56-1.61 and abbe number v dBe 39-52.
And in the compositing range of independent claim, has the barium flint glass that special equilibrated is formed, its optical data n by one group d, v dIn a close limit, change and have extraordinary chemical stability and extraordinary meltability and a processibility.Their compositing range (is the weight % of benchmark with the oxide compound) is as follows:
SiO 243-57; B 2O 37-11; BaO 11-26; CaO 0.1-0.5; ZnO 0-1.5; TiO 27.5-11; Al 2O 30.8-3; Na 2O 3.5-7; K 2O 3.5-7.5; Na wherein 2O+K 2O≤6.5;
The refractive index n of these glass dBe 1.57-1.61 and abbe number v dBe 43-48.
In order to improve the quality of glass, known one or more finingss of people can be joined in the mixture so that fining glass with common quantity.This glass has good especially inner glass quality, because it does not have bubble and crack.
If do not use As 2O 3As finings, and use Sb 2O 3Replace it, with regard to the quality of glass, it can accomplish and not have any loss, and not having lead glass according to the present invention also is no arsenic.
In another concrete scheme of the present invention, the glass that contains following finings can reach fabulous inner glass quality: the Sb of at least 0.05% weight 2O 3+ F -, the Sb of 0-0.5% weight wherein 2O 3And the F of 0-0.1% weight -For example the form with KF adds F -
Having positive abnormality according to glass of the present invention in the spectral range of blueness disperses to normal part.Explain:
Represented part dispersive ability in the spectrum of blue portion by following expression formula, promptly so-called relative part is disperseed.
P g . F = n g - n F n F - n c
" normal line " defined by following equation in the spectrum of blue spectrum
P g.F＝0.6438-0.001682·v d。
The glass that part disperses to be positioned on this line is referred to as " normal glass ".
Under the situation of glass with dispersion behavior different with " normal glass ", relevant P G.F-v dPoint leaves the ordinal number difference Δ P of " normal line " G.FAs described below:
Usually according to P G.FWhether " normal line " " above " (positive unusual part is disperseed) or " below " (negative unusual part is disperseed) be two classes with the glass rough segmentation.
Have unusual part dispersive glass to proofreading and correct remaining color effect, promptly so-called secondary spectrum is important.
Provide another group to have the lead-free optic glass of aforementioned optical characteristics according to glass compositing range of the present invention.Because these glass has been arranged, overcome the shortcoming of prior art, can not bring other shortcoming yet.
This glass has higher chemical stability and higher crystallization-stable.After a bit make in very large melting systems, for example producing glass in the optics melting area becomes possibility.This glass is fusing and processing easily therefore, and can economic production.
The fact that glass does not contain PbO is not only important because consider already mentioned environment protection, and because the density of glass reduces and the transition temperature increase of glass and positive effect is arranged.Another advantage is that this glass does not have As yet in preferred concrete scheme 2O 3
Embodiment:
Be fused into the glass of 8 embodiment of the present invention in preferred compositing range by common starting material.
Table 2 has provided composition separately (based on the weight % of oxide compound), refractive index n d, abbe number v d, the part in blue spectral range disperses P G.FWith this part dispersive changes delta P G.F, density p [g/cm 3], thermalexpansioncoefficient 20/300[10 -6/ K] and the transition temperature T of glass g[℃].
For embodiment 6-8, further measure the characteristic of glass, these represent that in table 3 especially put down in writing the chemical stability that high crystallization-stable (a kind of is to measure the crystalline fluid temperature) is become reconciled: this glass belongs to 1 grade of acid resistance, and specifically acid resistance is 1.0.They also belong to 1 grade of alkali resistance.In this case, along with B 2O 3/ (SiO 2+ TiO 2+ Al 2O 3) weight ratio reduce, alkali resistance from weight ratio be 0.19 o'clock 1.3 be changed to weight ratio be 0.12 o'clock 1.0.
Glass production of the present invention is as follows: the starting material that take by weighing oxide compound.Preferred carbonate and nitrate.Add finings Sb 2O 3, these are formed fully mix then.Under about 1340-1390 ℃, in the continuous melting system, this glass mixture is melted clarification and homogenizing then fully.Teeming temperature is 1180-1230 ℃.
Table 1 has been represented the embodiment of melt.
Table 1
Glass melt calculates with 100kg among the embodiment
Oxide compound Weight % Starting material Weight number [Kg]
SiO 2B 2O 3BaO TiO 2ZnO CaO Al 2O 3K 2O Na 2O Sb 2O 3 47.0 6.9 28.0 7.0 2.0 1.0 1.0 3.5 3.3 0.3 SiO 2 H 3BO 3 BaCO 3 TiO 2 ZnO CaCO 3 Al(OH) 3 K 2CO 3 KNO 3 NaHCO 3 Sb 2O 3 47.02 12.26 36.58 7.04 2.00 1.77 1.51 4.41 1.07 8.80 0.31
In table 2, provide the characteristic of the glass that obtains in this manner among the embodiment 3.
Table 2
The necessary characteristic of composition of glass (based on the weight % of oxide compound) and glass
1 2 3 4 5 6 7 8
SiO 2B 2O 3BaO CaO ZnO Al 2O 3TiO 2Na 2O K 2O Sb 2O 3n dv dP g.FΔP g.Fp[g/cm 3] α 20/300[10 -6/K] Tg[℃] 57.0 7.0 10.0 0.1 - 1.0 12.0 6.1 6.5 0.3 1.59106 43.11 0.5741 0.0028 2.74 7.81 586 58.5 8.0 10.0 0.1 - 1.5 7.0 7.1 7.5 0.3 1.59290 50.29 0.5596 0.0004 2.71 8.30 576 47.0 6.9 28.0 1.0 2.0 1.0 7.0 3.3 3.5 0.3 1.60887 47.82 0.5643 0.0010 3.15 7.94 607 42.0 6.9 28.0 1.0 2.0 1.0 12.0 3.3 3.5 0.3 1.64668 40.94 0.5781 0.0032 3.23 8.11 610 42.0 6.9 35.0 1.0 2.0 1.0 5.0 3.3 3.5 0.3 1.61464 49.91 0.5600 0.0002 3.32 8.80 593 55.7 7.6 11.6 0.3 1.3 1.0 9.0 6.5 6.9 0.3 1.58283 46.65 0.5663 0.0010 2.78 8.30 568 50.1 8.5 16.4 0.3 - 1.7 10.7 6.2 5.8 0.3 1.60585 43.69 0.5731 0.0028 2.88 8.32 577 44.6 10.7 25.6 0.1 - 2.8 8.1 4.0 3.8 0.3 1.60822 46.50 0.5678 0.0022 3.04 7.82 594
Table 3
The characteristic of the glass of embodiment 6-8
6 7 8
Acid resistance alkali resistance T (liquid) 60 minutes [℃/dPas] τ i400nm/25mm 1.0 1.0 840/1.47·10 5 0.887 1.0 1.2 995/1463 0.84 1.0 1.3 1025/800 0.794
In this table:
Acid resistance is according to ISO8424
Alkali resistance is according to ISO draft 10629
T (liquid) measures the fluid temperature and relevant viscosity of most fusing phases after 60 minutes 60 minutes
τ i400nm/25mm is the theoretical spectral transmissivity when wavelength X=400nm and thickness of sample d=25mm

Claims (8)

1. lead-free optical barium flint glass, its refractive index n dBe 1.55-1.66 and abbe number V dBe 39-52, it is characterized in that following composition (based on the weight % of oxide compound)
SiO 2 40-60
B 2O 3 6.5-12
BaO 10-35
CaO 0-1
ZnO 0-2
TiO 2 5-12
Al 2O 3 0.5-3.5
Na 2O 3-7.5
K 2O 3-8
And Na 2O+K 2O≤15
The common finings of quantity randomly.
2. according to the barium flint glass in the claim 1, its refractive index n dBe 1.60-1.66, it is characterized in that following composition (based on the weight % of oxide compound)
SiO 2 41-48
B 2O 3 6.5-8
BaO 28-35
CaO 0.5-1
ZnO 1-2
TiO 2 5-12
Al 2O 3 0.5-1.5
Na 2O 3-5
K 2O 3-5
And Na 2O+K 2O 6.5-8
The common finings of quantity randomly.
3. according to the barium flint glass in the claim 1, its refractive index n dBe 1.56-1.61, it is characterized in that following composition (based on the weight % of oxide compound)
SiO 2 46-59
B 2O 3 6.5-8.5
BaO 10-28
CaO 0.1-1
ZnO 0-2
TiO 2 6.5-12
Al 2O 3 0.5-2
Na 2O 3-7.5
K 2O 3-7.5
And Na 2O+K 2O 〉=6.5
The common finings of quantity randomly.
4. according to the barium flint glass in the claim 1, its refractive index n dBe 1.57-1.61 and abbe number v dBe 43-48, it is characterized in that following composition (based on the weight % of oxide compound)
SiO 2 43-57
B 2O 3 7-11
BaO 11-26
CaO 0.1-0.5
ZnO 0-1.5
TiO 2 7.5-11
Al 2O 3 0.8-3
Na 2O 3.5-7
K 2O 3.5-7.5
And Na 2O+K 2O≤14
The common finings of quantity randomly.
5. according to the barium flint glass of claim 1, it is characterized in that SiO 2, TiO 2And Al 2O 3Total amount be 47-72%.
6. according to claim 1,4 and 5 at least one barium flint glass, it is characterized in that B 2 O 3 Si O 2 + Ti O 2 + Al 2 O 3 Weight ratio be at most 0.20.
7. according to claim 1,4 and 5 at least one barium flint glass, it is characterized in that as finings, it contains (weight %):
Sb 2O 3 0-0.5
F 0-0.1
And F+Sb 2O 3〉=0.05
8. according to claim 1,4 and 5 at least one barium flint glass, it is characterized in that except unavoidable impurities it does not conform to arsenic oxide arsenoxide.
CN 98119951 1997-09-03 1998-09-03 Lead-free optical barium flint glass Expired - Lifetime CN1216822C (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE1997138428 DE19738428C1 (en) 1997-09-03 1997-09-03 New lead-free barium flint glass
DE19738428.5 1997-09-03

Publications (2)

Publication Number Publication Date
CN1214324A CN1214324A (en) 1999-04-21
CN1216822C true CN1216822C (en) 2005-08-31

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FR (1) FR2767814B1 (en)
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CN105819683B (en) * 2016-03-04 2019-12-03 成都光明光电股份有限公司 Environmental protection optical glass and optical element
CN110228945A (en) * 2019-06-28 2019-09-13 成都光明光电股份有限公司 A kind of optical glass and its gas preform, element and instrument
CN111320382A (en) * 2020-03-06 2020-06-23 成都光明光电股份有限公司 Optical glass
CN111533443B (en) * 2020-05-27 2022-04-15 成都光明光电股份有限公司 Optical glass

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FR2767814A1 (en) 1999-03-05
JP4213264B2 (en) 2009-01-21
DE19738428C1 (en) 1998-08-20
CN1214324A (en) 1999-04-21
GB2328937A (en) 1999-03-10
FR2767814B1 (en) 2000-06-23
JPH11171586A (en) 1999-06-29
GB9818277D0 (en) 1998-10-14
MY124577A (en) 2006-06-30

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