CN1990406B - Optical glass - Google Patents

Optical glass Download PDF

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Publication number
CN1990406B
CN1990406B CN2006101732657A CN200610173265A CN1990406B CN 1990406 B CN1990406 B CN 1990406B CN 2006101732657 A CN2006101732657 A CN 2006101732657A CN 200610173265 A CN200610173265 A CN 200610173265A CN 1990406 B CN1990406 B CN 1990406B
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Prior art keywords
glass
opticglass
sio
platinum
fusion
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CN1990406A (en
Inventor
佐藤史雄
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Nippon Electric Glass Co Ltd
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Nippon Electric Glass Co Ltd
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Publication of CN1990406A publication Critical patent/CN1990406A/en
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
    • 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
    • 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
    • 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
    • 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
    • C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum

Abstract

The objective of this invention is to provide a optical glass and producing method thereof, even melt raw glass material mixture which contains Sb as clarificant in melt device made of fire resisting material containing platinum, the optical glass can not reduce clarify effect and inhibit generation of platinum particle. The optical glass contains Sb and Sb<3+>/Sb at the ratio of more than 0.45.

Description

Opticglass
Technical field
The present invention relates to be used for the opticglass of lenss such as optical lens, solid-state imager.
Background technology
The opticglass of lenss such as solid-state imager that is used for optical lens and CCD, the CMOS etc. of the objective lens for optical pickup, pick up camera of CD, MD, DVD, other various optical disk systems and the imaging lens system of general camera etc.; Require it to have weathering resistance, do not contain particle and bubble etc., proposed the various glass of forming series.(for example with reference to patent documentation 1～5)
Patent documentation 1: TOHKEMY 2000-302479 communique
Patent documentation 2: TOHKEMY 2004-292306 communique
Patent documentation 3: TOHKEMY 2005-15302 communique
Patent documentation 4: TOHKEMY 2005-139023 communique
Patent documentation 5: japanese kokai publication hei 7-237933 communique
Summary of the invention
Because above-mentioned opticglass fusion under the temperature about 1000～1500 ℃ uses near this temperature, can emit clarification gas Sb composition as finings usually.And, owing to also require the height uniformity, in fusion apparatus, the general refractory materials that contains the Pt of heat and chemically stable, very difficult and glass reaction that uses.
But when using platiniferous refractory materials fusion opticglass, platinum melts the formation platinum grain in glass, and goes wrong.
Considering one of generation reason of platinum grain, is that Sb composition and the platinum as finings reacts.
Therefore,, consider to reduce Sb composition, and when reducing the Sb composition, residual bubble in glass becomes the critical defect as opticglass as finings as in order to suppress the method that platinum grain produces.
Suppress the method that platinum grain takes place as other; Consider to use the quartzy refractory materials of making to replace the method for platiniferous refractory materials melten glass; Yet quartz in melting process fused in the glass melting liquid and caused texture etc. this moment, and its result forms heterogeneous glass.
The object of the present invention is to provide a kind of opticglass; Even the fusion in the fusion apparatus of using the platiniferous refractory materials of this opticglass contains the frit mixture of Sb composition as finings; Clarifying effect can be do not reduced yet, and the platinum grain generation can be suppressed.
The inventor is through various researchs, and the result finds through in glass, increasing Sb 3+The ratio of/whole Sb just can not reduce clarifying effect so that fusion contains the frit mixture of Sb composition as finings in the fusion apparatus of using the platiniferous refractory materials yet, and can suppress the platinum grain generation, has finally proposed the present invention.
That is, the present invention relates to following (1)～(11).
(1) a kind of opticglass contains the Sb composition, wherein, and Sb 3+/ all the ratio of Sb is more than 0.45.
(2) like above-mentioned (1) described opticglass, the Sb composition is converted into Sb 2O 3After content be 0.02～2 weight %.
(3) like above-mentioned (1) described opticglass, the dissolved amount of oxygen is below the 70 μ l/g in glass.
(4) like above-mentioned (1) described opticglass, be SiO 2-B 2O 3-RO-R ' 2O is that (R representes more than one among Mg, Ca, Sr, the Ba to glass, more than one among R ' expression Li, Na, the K.)。
(5) like each described opticglass in above-mentioned (1)～(4),, contain SiO in weight percent 220～60%, B 2O 32～30%, RO 5～30%, R ' 2O 1～15%.
(6) like above-mentioned (1) described opticglass, be SiO 2-B 2O 3-RO-R ' 2O-R " 2O 3Be glass (R " among expression Y, La, the Gd more than one.)。
(7) like each described opticglass in above-mentioned (1)～(3) and (6),, contain SiO in weight percent 220～60%, B 2O 32～40%, RO 5～30%, R ' 2O 1～15%, R " 2O 31～40%.
(8) like above-mentioned (1) described opticglass, be SiO 2-B 2O 3-R ' 2O-TiO 2-Nb 2O 5Be glass.
(9) like each described opticglass in above-mentioned (1)～(3) and (8),, contain SiO in weight percent 220～60%, B 2O 32～30%, R ' 2O 1～15%, TiO 21～25%, Nb 2O 51～25%.
(10) like above-mentioned (1) described opticglass, be B 2O 3-ZnO-R " 2O 3Be glass.
(11) like each described opticglass in above-mentioned (1)～(3) and (10),, contain B in weight percent 2O 310～45%, ZnO 5～50%, R " 2O 310～50%.
The invention effect
According to the present invention, can obtain as causing light platinum grain and the less opticglass of bubble with the image deflects reason at random.Therefore, be suitable as opticglass.
Embodiment
When fusion contains the Sb composition as the frit mixture of finings in the fusion apparatus of using the platiniferous refractory materials, consider that generally it is the reason that platinum grain is separated out in the glass that Sb composition and platinum react.As the Sb composition of finings, in glass melting liquid with Sb 5+And Sb 3+State exist.Sb 5+Part valence mumber under the temperature more than 1000 ℃ change and to become Sb 3+, meanwhile emit oxygen and help the clarification of glass, the Sb that valence mumber changes does not take place 5+With platinum reactive etching platinum, the result separates out platinum grain in glass.In addition, the Sb that in glass, exists 5+Content after a little while, though can suppress the generation of platinum grain, can reduce clarifying effect.For this reason, want to make clarifying effect not reduce and reduce the generation of platinum grain, control is the Sb more than the necessary amount for clarification 5+Just very important.
The inventor attentively studies, if the result finds Sb in making the glass that finally obtains 3+/ all the ratio of Sb is fusion under the condition more than 0.45; Then can be on the basis that produces for the sufficient oxygen of clarification; Suppress the generation of platinum grain; In addition, be fusion under the condition below the 70 μ l/g through dissolved oxygen amount in making glass, can more effective inhibition platinum grain and the generation of bubble.
Sb in the glass that finally obtains 3+/ all the ratio of Sb diminishes, that is, and and Sb 5+Ratio increase, mean in the glass melting operation Sb 5+Valence mumber variation becoming Sb does not further take place 3+, this generation with platinum grain and bubble is relevant.Sb 3+/ all the ratio preferred range of Sb is more than 0.50, preferred scope is more than 0.55, the scope that is more preferably is more than 0.60.
In addition, dissolved oxygen amount increases in the glass that finally obtains, and is because the dissolved oxygen amount that in glass, can allow reduces, and delicate variation takes place the glass melting condition, therefore from Sb 5+Valence mumber variation becoming Sb takes place 3+The process easy interruption, relevant with the generation of platinum grain and bubble.Dissolved oxygen amount preferred range is that 65 μ l/g are following, preferred scope is that 50 μ l/g scope following, that be more preferably is below the 40 μ l/g in the glass.
In addition, make Sb in the glass 3+/ all the ratio of Sb becomes big, in the glass quantitative change of dissolved oxygen little, can adopt and for example improve melt temperature, prolong the method for fusion time etc.In addition, when using the continuous fusion stove to carry out plant-scale production, obtain the Sb in the glass that obtains 3+Ratio and the dissolved oxygen amount of/whole Sb can change operational conditions so that Sb according to these values 3+/ all ratio and the dissolved oxygen amount of Sb are suitable value.
In addition, in opticglass, require to have height uniformity and strict specific refractory power; As the method for making such glass, have in advance glass melting is made, its pulverizing; The sheet glass after pulverizing (when specific refractory power is adjusted into precision; Melting making has the glass of the specific refractory power higher than targeted refractive index and the glass with specific refractory power lower than targeted refractive index respectively, and these glass are pulverized, and the sheet glass after pulverizing is mixed making it to have targeted refractive index) fused method again.When making opticglass, want to make the Sb in the glass with aforesaid method 3+/ all the ratio of Sb becomes big; The quantitative change of dissolved oxygen is little in the glass; Also can be employed in advance and to contain Sb composition and fusion at high temperature in the glass of making, will prolong the fusion time, the sheet glass after will pulverizing under the temperature that perhaps melt temperature than previous manufacturing glass the time is low is method such as fusion again.Thus, in the time of can being suppressed at fusion and the again generation of platinum grain and bubble during fusion.
Method of manufacture in the face of opticglass of the present invention describes down.
At first, as finings, prepare to contain the frit mixture of Sb composition.The content of Sb composition preferably is converted into Sb with the Sb composition in the glass that finally obtains 2O 3Be that 0.02～2 weight % mixes.When its content reduces, be difficult to obtain sufficient clarifying effect.On the other hand, content for a long time, glass coloring is with the Sb of platinum reaction 5+Ratio increase.Sb 2O 3Preferred scope is 0.02～1.5 weight %, and the scope that is more preferably is 0.02～0.5 weight %.In addition, preferably use the Sb oxide compound, the Sb oxide compound (Sb of 3 valencys that preferred especially use and platinum are difficult to react as the Sb composition 2O 3).Need to prove that so long as do not corrode the degree of platinum, the finings except the Sb oxide compound can also use for example Sn oxide compound, As oxide compound.
In addition, as glass, so long as satisfy the opticglass of various characteristicses such as desired anti-increased devitrification resistance, weathering resistance in the lens purposes, just not special restriction, but especially preferably use SiO 2-B 2O 3-RO-R ' 2O is glass, SiO 2-B 2O 3-RO-R ' 2O-R " 2O 3Be glass, SiO 2-B 2O 3-R ' 2O-TiO 2-Nb 2O 5Be glass or B 2O 3-ZnO-R " 2O 3Be glass.Here, R representes more than one among Mg, Ca, Sr, the Ba, more than one among R ' expression Li, Na, the K, R " among the expression Y, La, Gd more than one.
Using SiO 2-B 2O 3-RO-R ' 2When O is glass, in weight percent, preferably to have SiO 220～60%, B 2O 32～30%, RO 5～30%, R ' 2The composition hybrid glass raw material of O 1～15%.
Using SiO 2-B 2O 3-RO-R ' 2O-R " 2O 3When being glass, in weight percent, preferably to have SiO 220～60%, B 2O 32～40%, RO 5～30%, R ' 2O 1～15%, R " 2O 31～40% composition hybrid glass raw material.
Using SiO 2-B 2O 3-R ' 2O-TiO 2-Nb 2O 5When being glass, in weight percent, preferably to have SiO 220～60%, B 2O 32～30%, R ' 2O 1～15%, TiO 21～25%, Nb 2O 51～25% composition hybrid glass raw material.
Using B 2O 3-ZnO-R " 2O 3When being glass, in weight percent, preferably to have B 2O 310～45%, ZnO 5～50%, R " 2O 310～50% composition hybrid glass raw material.
The frit mixture fusion that then, will have above-mentioned composition.At this moment, the Sb in making the glass that finally obtains 3+/ all the ratio of Sb be more than 0.45, preferably more than 0.50, be more preferably more than 0.55, be more preferably be under the condition more than 0.60 and in making glass dissolved oxygen amount be below the 70 μ l/g, preferably below the 65 μ l/g, be more preferably below the 50 μ l/g, the scope that is more preferably is that to carry out fusion under the condition below the 40 μ l/g be very important.
Need to prove that melting making contains the glass of Sb in advance, it is pulverized, use sheet glass after pulverizing as the frit mixture, when opticglass is made in fusion again, the also Sb in making the glass that finally obtains 3+It also is very important carrying out fusion under the condition of dissolved oxygen amount in above-mentioned scope in the ratio of/whole Sb, the glass.
Afterwards, through melten glass being configured as certain shape, can obtain Sb 3+/ all the ratio of Sb is more than 0.45, the opticglass that subsurface defects such as bubble, platinum grain are less.In addition, manufacturing process can suitably be selected to use according to purposes, for example, as die pressing optical glass the time, can suitably use drop forming method etc.
Embodiment
Below based on embodiment the present invention is described.
Table 1 expression embodiments of the invention (sample No.1～3) and comparative example (sample No.4,5).
Table 1
1 2 3 4 5
The melting condition melt temperature (℃) fusion time (hr) again melt temperature (℃) 1,300 10 1300 1,200 10 1200 1,200 1 1200 1,150 10 1200 1,150 10 1100
Sb 3+/ whole Sb 0.70 0.63 0.56 0.40 0.35
Dissolved oxygen amount (μ l/g) 21.4 31.5 55.5 71.4 81.0
Platinum grain A A B C B
Bubble a a a a b
In experiment, used in weight percent to have by SiO 250%, Al 2O 33%, B 2O 310%, CaO 6%, SrO 8%, BaO 11%, ZnO 3%, Li 2O 7%, Na 2The essentially consist that O2% forms, and added 0.2% Sb oxide compound (Sb 2O 3) as the SiO of finings 2-B 2O 3-RO-R ' 2O is a glass.
Each sample is according to preparing as follows.At first, the hybrid glass raw material makes it into as above forming it to be filled to the crucible of platinum system and to put into electric furnace, fusion under the melting condition that it is as shown in the table.Afterwards, from electric furnace, take out crucible, make the glass melting flow to carbon plate, glass block is made in cooling.Then glass block is pulverized, made the sheet glass that size is about 5mm.Be filled to the sheet glass 50g that makes in the crucible of platinum system then and put into electric furnace, fusion is 5 hours under the melt temperature again that it is as shown in the table.Afterwards, from electric furnace, take out crucible, make the glass melting flow to carbon plate, further the annealing back makes and is fit to the sample that each is measured.
Sb in the sample that mensuration obtains 3+Remaining platinum grain and bubble in the ratio of/whole Sb, dissolved oxygen amount, the glass.Its result is as shown in table 1.
Can know from table 1, in each sample of embodiment of the invention No.1～3, Sb 3+/ all the ratio of Sb is more than 0.56, dissolved oxygen amount is below the 55.5 μ l/g.And platinum grain and bubble remaining in the glass are less.
Relative therewith, in comparative example sample No.4 and No.5, Sb 3+/ all the ratio of Sb is below 0.40, dissolved oxygen amount is that platinum grain remaining in the glass among the sample No.4 is more more than the 71.4 μ l/g, and bubble remaining in the glass among the No.5 is more.
In addition, obtain Sb through following method 3+The ratio of/whole Sb.Utilize sulfuric acid and hydrofluoric acid, potassium permanganate thermal degradation glass powder, in hydrochloric acid, after the dissolving, use the ICP-AES device to carry out quantitatively all Sb.In addition, at first in inert gas atmosphere, in glass powder, add hydrochloric acid and hydrofluoric acid, make its decomposition through ten minutes heat (water-bath).Then, add Na 2CO 3, with the hydrofluoric acid neutralization of surplus, for preventing Sb 3+Hydrolysis adds tartrate NaK, NaHCO 3, make it convert solubility double salt into after, end to import rare gas element.Afterwards, add Starch Indicator, with the titration of N/100 iodine solution, quantitative analysis Sb 3+Obtain Sb like this 3+With whole Sb, calculate Sb 3+The ratio of/whole Sb.
Dissolved oxygen amount is that the about 1g of sample is warming up to 500～1400 ℃ with the speed of 8 ℃/min, measures the total amount of the amount of oxygen of emitting.In addition, helium is used in carrier gas, feeds with flow 50ml/min.
For platinum grain remaining in glass and bubble, making size is the thick sample of 30 * 30 * 20mm, measures with stereoscopic microscope (30 times).In addition, for platinum grain, with in every gram glass be below 0.5 as " A ", 0.5～4 as " B ", surpass 4 and estimate as " C ".In addition, for bubble, with in every gram glass below 2 as " a ", surpass 2 estimate as " b ".

Claims (6)

1. SiO 2-B 2O 3-RO-R ' 2O system, SiO 2-B 2O 3-RO-R ' 2O-R " 2O 3System, SiO 2-B 2O 3-R ' 2O-TiO 2-Nb 2O 5System or B 2O 3-ZnO-R " 2O 3Be opticglass, contain the Sb composition, it is characterized in that Sb 3+/ all the ratio of Sb is more than 0.45, the dissolved amount of oxygen is that wherein R representes more than one among Mg, Ca, Sr, the Ba below the 70 μ l/g in glass, more than one among R ' expression Li, Na, the K, R " and among the expression Y, La, Gd more than one.
2. opticglass as claimed in claim 1, the Sb composition is converted into Sb 2O 3After content be 0.02～2 weight %.
3. according to claim 1 or claim 2 opticglass, said opticglass is SiO 2-B 2O 3-RO-R ' 2When O is opticglass,, contain SiO in weight percent 220～60%, B 2O 32～30%, RO 5～30%, R ' 2O 1～15%.
4. according to claim 1 or claim 2 opticglass, said opticglass is SiO 2-B 2O 3-RO-R ' 2O-R " 2O 3When being opticglass,, contain SiO in weight percent 220～60%, B 2O 32～40%, RO 5～30%, R ' 2O 1～15%, R " 2O 31～40%.
5. according to claim 1 or claim 2 opticglass, said opticglass is SiO 2-B 2O 3-R ' 2O-TiO 2-Nb 2O 5When being opticglass,, contain SiO in weight percent 220～60%, B 2O 32～30%, R ' 2O 1～15%, TiO 21～25%, Nb 2O 51～25%.
6. according to claim 1 or claim 2 opticglass, said opticglass is B 2O 3-ZnO-R " 2O 3When being opticglass,, contain B in weight percent 2O 310～45%, ZnO 5～50%, R " 2O 310～50%.
CN2006101732657A 2005-12-28 2006-12-15 Optical glass Active CN1990406B (en)

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JP2005377469A JP2007176748A (en) 2005-12-28 2005-12-28 Optical glass
JP2005-377469 2005-12-28
JP2005377469 2005-12-28

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Publication number Priority date Publication date Assignee Title
JP5729532B2 (en) * 2008-10-07 2015-06-03 日本電気硝子株式会社 Optical glass
JP5850384B2 (en) * 2009-04-17 2016-02-03 日本電気硝子株式会社 Glass
CN107162427B (en) 2017-03-24 2019-01-11 中山大学 A kind of high power semiconductor light source activation glass ceramics and its preparation method and application

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US20050143247A1 (en) * 2000-04-08 2005-06-30 Schott Glas Flat float glass

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JP2004269347A (en) * 2003-02-18 2004-09-30 Nippon Electric Glass Co Ltd Glass composition
JP2005162600A (en) * 2003-11-11 2005-06-23 Nippon Electric Glass Co Ltd Cover glass plate for semiconductor package
EP1604959A1 (en) * 2004-06-02 2005-12-14 Kabushiki Kaisha Ohara An optical glass
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CN1105955A (en) * 1993-11-26 1995-08-02 株式会社小原 Optical glass
US20050143247A1 (en) * 2000-04-08 2005-06-30 Schott Glas Flat float glass
CN1374265A (en) * 2001-02-20 2002-10-16 保谷株式会社 Optical glass, mould pressing preshaping piece and optical components

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D.M.Krol,P.J.Rommers.Oxidation-reduction behaviour of antimony in silicate glasses prepared from raw materials and cullet.《Glass Technology》.1984,第25卷(第2期),第115页左栏第1-2段、右栏最后1段,表1. *

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