CN101296872A - Optical glass, apparatus for producing optical glass, and process for producing the same - Google Patents
Optical glass, apparatus for producing optical glass, and process for producing the same Download PDFInfo
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- CN101296872A CN101296872A CNA2006800401496A CN200680040149A CN101296872A CN 101296872 A CN101296872 A CN 101296872A CN A2006800401496 A CNA2006800401496 A CN A2006800401496A CN 200680040149 A CN200680040149 A CN 200680040149A CN 101296872 A CN101296872 A CN 101296872A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
An optical glass which has excellent unsusceptibility to solarization and is prevented from generating platinum knots. The optical glass contains, in terms of mass%, 30 to 70% SiO2 and/or 3 to 20% B2O3 and has a platinum content of 5 ppm or lower. Also provided is a process for producing the optical glass using a melting apparatus, wherein the gas inside the apparatus is replaced at a rate of 2 to 20 times per minute in terms of the capacity of the melting furnace and a non-oxidizing gas is bubbled into the molten glass.
Description
Technical field
The present invention relates to the SiO that contains of a kind of ageing-resistant (solarization resistance) excellent performance
2And/or B
2O
3Opticglass, make when stirring melts and contain SiO by advertising gas (bubbling)
2And/or B
2O
3Opticglass manufacture method, make when discharging the gas in the melting plant and contain SiO
2And/or B
2O
3Opticglass manufacture method and make and to contain SiO
2And/or B
2O
3The device of opticglass.
Background technology
When making opticglass, importantly in making multiple frit fused glass cullet chemical industry preface and/or formal fusion operation, melts (raw glass or glass) is fully stirred.As the method that stirs melts, provide with agitating wing and stirred the mechanical mixing method of melts and the method for advertising (for example, with reference to patent documentation 1) that using gas is advertised device.Herein, the method for advertising is meant such method: in fusion tank or the bottom of fusion tank configuration gas advertise device, advertise the bubble that device is blown into gas such as oxygen from gas, make liquid move along with the rising of bubble, come stirred liq with this.
And, want production quality in high yield ground very uniformly during opticglass in desire, must prevent to advertise the pollution (contamination) of melting plants such as device or fusion tank from described gas.Therefore, in general using what contact with melts at least partly or entirely is the melting plant that platinum or platinum alloy constituted by thermotolerance and excellent corrosion resistance.
Patent documentation 1: the special public clear 48-27724 communique of Japanese Patent
Yet when fusion tank or gas were advertised device etc. and used platinum or platinum alloy, the high temperature the when part of platinum part or platinum alloy part can be because of fusion reacted with airborne oxygen, thereby generates platinum dioxide (PtO
2).This PtO
2Can become gas, and fuse into the melten glass via molten glass surface from gas phase.And, platinum ion (Pt
4+) also can be from containing SiO
2And/or B
2O
3Melten glass and the boundary surface of platinum or platinum alloy fuse in the melten glass.It is generally acknowledged to have some cognation between platinum ion and the catabiosis, for example, contain SiO when fusing into
2And/or B
2O
3Melten glass in Pt
4+(contain PtO
2) remain in the finished product as impurity be in the opticglass time, cause sometimes and contain SiO
2And/or B
2O
3The transmissivity of glass worsen or be accompanied by the catabiosis of uviolizing.
Described catabiosis can make and contain SiO
2And/or B
2O
3The degradation of optical lens, so can suppress catabiosis, become the important factor that adopts this optical lens.For example, for the optical lens of i line stepper, require it that catabiosis that causes because of uviolizing can not take place.
Although there is the problem of aforesaid catabiosis, in pyritous glass is made, because aforesaid reason will use the fusion tank of platinum system or platinum alloy system or gas to advertise device inevitably.Therefore, expect a kind of SiO that contains of ageing-resistant performance excellence
2And/or B
2O
3Opticglass.
Summary of the invention
The present invention develops in view of aforesaid problem, and purpose is to provide a kind of SiO that contains of ageing resistance excellence
2And/or B
2O
3Opticglass and being used for make the ageing resistance excellence glass contain SiO
2And/or B
2O
3The manufacture method and the manufacturing installation of opticglass.
Particularly, the invention provides following content.
(1) a kind of opticglass, it contains SiO
2And/or B
2O
3, this opticglass is characterised in that Pt content (quality criteria) wherein is below the 5ppm.
(2) according to (1) described opticglass, it is characterized in that come in mass percent, described opticglass contains the SiO more than 30%, below 70%
2And/or 3% above, B below 20%
2O
3
(3) according to (1) or (2) described opticglass, it is characterized in that,
Come in mass percent, described opticglass contains following compositions:
(a) SiO
2: 30～70% and/or
B
2O
3: 3～20% and/or
PbO:0～2% and/or
Al
2O
3: 0～6% and/or
Li
2O:0～5% and/or
CaO:0～2% and/or
TiO
2: 0～0.5% and/or
As
2O
3: 0～1% and/or
Sb
2O
3: 0～1% and/or
Na
2O:0～13% and/or
K
2O:0～23% and/or
BaO:0～42% and/or
ZnO：0～7％
And
(b) the total amount of part or all of described oxide compound F in the fluorochemical of displacement gained is 0～11%.
(4) according to each described opticglass in (1) to (3), it is characterized in that, come Na in mass percent
2O+K
2O+BaO+ZnO is 10～45%.
According to each described opticglass in (1) to (4), it is characterized in that (5), come that SrO is 0～2% and/or ZrO in mass percent
2Be 0～2%.
(6) according to each described opticglass in (1) to (5), it is characterized in that, come CaO+SrO+ZrO in mass percent
2Be 0～2%.
(7) according to each described opticglass in (1) to (6), it is characterized in that come in mass percent, described opticglass contains 50.5～70% described SiO
2, 3～15% described B
2O
3, the described Al below 2.9%
2O
3And the described Li below 4.9%
2O.
(8) according to each described opticglass in (1) to (7), it is characterized in that come in mass percent, described opticglass contains 55.35～70% described SiO
2, the described Al below 2.3%
2O
3And the described Li below 3%
2O.
(9) according to each described opticglass in (1) to (8), it is characterized in that the total content (quality criteria) of V, Cr, Mn, Fe, Co, Ni, Cu, Ag, W, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Dy, Ho, Fr, Tm, Yb, each composition of Lu is below the 3ppm.
(10) a kind of manufacture method of opticglass, it comprises following operation: " with raw mix (below be called batch of material) fusion and obtain the operation (below be called glass cullet chemical industry preface) of glass cullet " and/or " with glass cullet and/or batch of material fusion and obtain the operation (below be called formal fusion operation) of glass ", the manufacture method of described opticglass is characterised in that
Contain SiO in the composition of the glass that is obtained
2And/or B
2O
3, and
In the melts of described glass cullet chemical industry preface and/or described formal fusion operation, advertise non-oxidizing gas.
(11) according to the manufacture method of (10) described opticglass, it is characterized in that, described non-oxidizing gas is blown into apart from the degree of depth more than the liquid level 100mm of described melts.
(12) according to the manufacture method of (10) or (11) described opticglass, it is characterized in that, be blown into described non-oxidizing gas with 0.002～0.05 liter/minute feed speed at per 1 liter of glass volume.
(13) according to the manufacture method of each described opticglass in (10) to (12), it is characterized in that described non-oxidizing gas is He, Ne, Ar, Kr, Xe, N
2, H
2, CO or these gases various mixed gases.
(14) a kind of manufacture method of opticglass, it comprises following operation: will " raw mix (below be called batch of material) fusion and obtain the operation (below be called glass cullet chemical industry preface) of glass cullet " and/or " described glass cullet and/or batch of material fusion being obtained the operation (below be called formal fusion operation) of glass ", the manufacture method of described opticglass is characterised in that
Contain SiO in the composition of the glass that is obtained
2And/or B
2O
3System, and
Gas in the space in the melting plant in described glass cullet chemical industry preface and/or the described formal fusion operation is discharged.
(15) manufacture method of basis (14) described opticglass, it is characterized in that, in described glass cullet chemical industry preface and/or described formal fusion operation, make described batch of material and/or described glass cullet fusion, simultaneously the gas in the space in the described melting plant is discharged with it.
(16) according to the manufacture method of (14) or (15) described opticglass, it is characterized in that, is benchmark with the spatial volume in the described melting plant, replaces gas in this melting plant with 2～20 times/minute speed.
(17) a kind of manufacturing installation of opticglass, described opticglass contains SiO at least
2And/or B
2O
3, the manufacturing installation of this opticglass is characterised in that,
Comprise: the batch of material fusion is obtained the batch of material melting plant of glass cullet and/or described glass cullet or described batch of material fusion are obtained the formal melting plant of glass melting thing, the non-oxidizing gas bubbling device is arranged in the described raw mix melting plant and/or in the described glass cullet melting plant.
(18) a kind of manufacturing installation of opticglass, described opticglass contains SiO at least
2And/or B
2O
3, the manufacturing installation of this opticglass is characterised in that,
Comprise: fusion tank is used for making batch of material or glass cullet fusion and obtains melts; Body of heater, cover described fusion tank around, and have the peristome that drops into described batch of material or described glass cullet; And air-releasing mechanism, its configuration or connection are used for the gas that described melts produced in the described fusion tank is discharged near described peristome.
The effect of invention
According to the present invention, can provide a kind of SiO that contains of ageing resistance excellence
2And/or B
2O
3Opticglass.
According to the manufacture method of opticglass of the present invention, can provide a kind of and use platinum or platinum alloy in the fusion operation as the melting plant of material, can suppress the manufacture method of the opticglass of catabiosis or generation platinum plethora.
Its result can obtain before unexistent " the initial stage light transmittance is good " and/or the opticglass of " light transmittance after the irradiate light worsens less ", uses the opticglass that uses in the various fields such as (especially stepper is used), physiotechnology or medical treatment as semiconductor industry.
Description of drawings
Fig. 1 (A) is the orthographic plan with frit fused raw materials melt device.Fig. 1 (B) is the orthographic plan that makes the formal melting plant of glass cullet fused.
Fig. 2 (A) is to use the gas of embodiment of the present invention to advertise the sectional view along the IV-IV of Fig. 1 (A) of the batch of material melting plant of device.Fig. 2 (B) is to use the gas of embodiment of the present invention to advertise the sectional view along the IV-IV of Fig. 1 (B) of the formal melting plant of device.
Fig. 3 is deterioration rate graphic of the transmissivity of expression i line irradiation time and opticglass.
The explanation of symbol
100 batch of material melting plants
200 formal melting plants
102,202 melting furnaces
106,206 gases are advertised device
110,210 air interchangers
112,212 conus portions
114,214 suction ports
116,216 vapor pipes
121,221 fusion tanks
122,222 bodies of heater
126,226 peristomes
203 relief outlets
204 transfer limes
A batch of material melts
The formal melts of D
Embodiment
Below, according to the graphic the embodiments of the present invention that illustrate.In addition, in the following description of the embodiment, identical component parts has been marked same-sign, and omitted or simplify its explanation.
Moreover the present invention is not limited to following illustrated embodiment, and the distortion in the scope that can realize the object of the invention, improvement etc. all belong to the present invention.
The composition of glass
The compositing range that constitutes each composition of opticglass of the present invention will be in following description.Each composition is expressed with mass percent.In addition, the expressed glass composition of mass percent all is to be expressed by the mass percent that is benchmark with the oxide compound in the application's case specification sheets.Herein " is benchmark with the oxide compound " to be supposition all decompose when fusion when becoming oxide compound as the oxide compound of the raw material of glass constituent of the present invention, nitrate etc., the quality summation of the oxide compound that generated is made as 100 mass percents, and then the composition of each composition that is contained in the statement glass:.
At first, the SiO that contains that can make the ageing resistance excellence among the present invention is described
2And/or B
2O
3Opticglass, especially SiO
2-B
2O
3The compositing range of the opticglass of composition.
Each composition is defined as the reasons are as follows of described compositing range.
For containing SiO
2Opticglass, SiO
2It is useful composition aspect glass formation.But, work as SiO
2Weight percent not preferred less than 30% o'clock because cause the B that needs more amount easily this moment
2O
3Or the tendency of composition such as BaO, specific refractory power also uprises easily in addition, perhaps causes chemical property to worsen easily.In addition, if SiO
2Surpass 70%, then the viscosity of glass uprises easily, and the result causes being difficult to obtain the uniform glass of quality easily.Therefore, consider the deterioration characteristics of specific refractory power, chemical property, the factors such as viscosity of glass, thus SiO
2Lower limit preferred more than 50.5%, more preferably more than 53.0%, most preferably more than 55.35%.And, SiO
2The upper limit preferred below 70%, more preferably below 65%, most preferably below 61%.
For containing B
2O
3Opticglass, B
2O
3With SiO
2Be the oxide compound that forms glass equally, make the low chromatic dispersionization of glass or regulating aspect the viscosity effective.But, work as B
2O
3Less than 3% and surpass 20% o'clock not preferred, this be because, if B
2O
3Less than 3%, then easily make its effect insufficient, and if above 20%, then chemical property worsens easily.Further contemplate low chromatic dispersion, the viscosity of glass, the factors such as deterioration of chemical property, thus B
2O
3Preferred more than 3%, below 20%.Therefore, B
2O
3The upper limit preferred below 20%, more preferably below 17%, most preferably below 15%.And, B
2O
3Lower limit preferred more than 3%, more preferably more than 5%, most preferably more than 6%.
Al
2O
3Effective aspect the chemical durability that improves glass, adjustment viscosity or specific refractory power.But, work as Al
2O
3Surpass at 6% o'clock, the viscosity of glass uprises easily.And, further contemplate the factors such as chemical durability, viscosity or specific refractory power of glass, thus Al
2O
3More preferably below 2.9%, most preferably below 2.3%.
Li
2O has the frit of promotion fused effect, compares with other alkali metal oxide compound, is difficult to cause specific refractory power to reduce, so be effective composition.But, work as Li
2O is not preferred above 5% o'clock, because cause this moment the increased devitrification resistance of glass to increase easily.And, further contemplate the factors such as deterioration of viscosity, specific refractory power, chemical property, thus Li
2O is more preferably below 4.9%, most preferably below 3%.
Na
2O and K
2O is effective aspect the fusion that promotes frit, even if contain Na in the glass in a large number
2O and K
2O also can make stable glass.But, work as Na
2O and K
2The amount of O surpass respectively 13% and 23% o'clock not preferred because cause this moment chemical property to worsen easily.Na
2The upper limit of O is preferred below 13%, more preferably below 10%, most preferably below 7%.And, K
2The upper limit of O is preferred below 23%, more preferably below 20%.
BaO can excessively not increase the chromatic dispersion (can excessively not reduce Abbe number) of glass, but can improve specific refractory power, can obtain the bigger stable glass of devitrification resistance in wider compositing range.But if BaO surpasses 42%, then the chemical durability of glass extremely worsens easily.Therefore, the upper limit of BaO is preferred below 42%, more preferably below 25%, most preferably below 18%.
ZnO is improving specific refractory power, is adjusting viscosity, is improving the effective composition in aspect such as devitrification resistance.But, not preferred when ZnO surpasses 7%, because can cause this moment the transmissivity in short wavelength zone to descend.Therefore, the upper limit of ZnO is preferred below 7%, more preferably below 3%, most preferably below 1%.
Again, for obtain to stablize, chemical property excellence and all good glass of the transmissivity till the short wavelength zone, Na
2O, K
2The upper limit of the scope (%) of the total amount of one or more compositions of O, BaO and ZnO is preferred below 45%, more preferably below 40%, most preferably below 35%.And lower limit is preferred more than 10%, more preferably more than 13%, most preferably more than 15%.
PbO and TiO
2For containing SiO
2And/or B
2O
3Opticglass, particularly for SiO
2-B
2O
3-alkalimetal oxide and/or alkaline-earth metals oxide are glass, prevent aspect the catabiosis effective.But if the content of described composition, then becomes the reason of the light transmittance deterioration that causes the short wavelength zone easily above required, therefore, the upper limit of the content of described composition is preferred respectively below 2% and below 1.0%, more preferably below 1% and below 0.1%.
As
2O
3And Sb
2O
3Have effect, can distinguish at random and add, but, add below 1% just enough respectively in order to obtain described effect as the glass clarifying auxiliary agent.
Fluorine can be used as and carries out the metathetical fluorochemical with part or all of one or more described oxide compounds and add arbitrarily, adjust aspect specific refractory power and the viscosity effective.But not preferred when the total amount of described fluorochemical surpasses 11%, because the easy opacification of glass this moment, perhaps specific refractory power becomes too small easily, excessively volatilization of fluorine when fusion, thus be difficult to make the uniform glass of quality.The upper limit of the total amount of fluorochemical is preferred below 11%, more preferably below 9.5%.
In addition, except described each composition,, can also add being no more than 2% any composition CaO, SrO and ZrO respectively in order to adjust specific refractory power and to improve chemical property of glass etc.
2Moreover, when adding these compositions, be selected from CaO, SrO and ZrO
2In one or more total amount preferably be no more than 2%, more preferably below 1%.
And the transition metal beyond the Ti is for example below the preferred 3ppm of total content of V, Cr, Mn, Fe, Co, Ni, Cu, Ag, W, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Dy, Ho, Fr, Tm, Yb, each composition of Lu.The uptake factor of described each composition that contains as impurity is bigger, also can cause transmissivity to worsen even if sneak on a small quantity.
In order to prevent catabiosis, below the preferred 5ppm of Pt content of opticglass of the present invention.Below the further preferred 1ppm, more preferably below the 0.5ppm, most preferably below the 0.2ppm.
Batch of material melting plant, glass cullet chemical industry preface
Below, describe the batch of material fusing device, the glass cullet chemical industry preface that are used for making the good glass of the less and ageing-resistant phenomenon of platinum content in detail.
Shown in Fig. 1 (A) and Fig. 2 (A), the batch of material melting plant 100 that uses in the glass cullet chemical industry preface comprises: melting furnace 102 is used for making the batch of material fusion to obtain batch of material melts A; And gas advertises device 106, advertises gas in described batch of material melts A.And melting furnace 102 comprises: the fusion tank 121 of the container when becoming the batch of material fusion; Cover this fusion tank 121 body of heater 122 on every side; And heating unit (not shown).
For fusion tank 121, consider batch of material melts A fusion, the required thermotolerance of clarification, anti-erosion is given birth to and to factors such as the quality influence of batch of material melts A are less, preferably, at least the part that contacts with batch of material melts A for example is the fusion tank that is made of quartz, platinum (Pt) or platinum alloy (Pt alloy), the more preferably fusion tank 121 that is made of platinum or platinum alloy.
Around the body of heater 122 covering fusion tanks 121, formed by heat-stable materials such as refractory brick.On the top of this body of heater 122, formed in order in fusion tank 121, to drop into the peristome 126 of frit.And peristome 126 becomes in order to remaining gas in the batch of material melts A in the fusion tank 121 is imported to the inlet of discharger (not shown), and described discharger is connected in from body of heater 122 inner air interchangers 110 of discharging described survival gas.
Gas is advertised device 106 and is inserted in the fusion tank 121 from described peristome 126.That is, the peristome 126 double as gas that is used for advertising gas in melts is advertised the patchhole of device 106.In order fully to stir batch of material melts A, the structure that gas is advertised device 106 is the well-known structure that can produce larger bubbles as much as possible.For this gas is advertised device 106, consider their thermotolerance, to the erosion resistance of batch of material melts A and to factor such as the influence of the quality of batch of material melts A is less, preferably, for example the part that contacts with batch of material melts A is to advertise device by the gas that quartz, platinum or platinum alloy constitute, and more preferably the gas that is made of platinum or platinum alloy is advertised device.
When the member or the gas of formation batch of material melting plants 100 such as fusion tank 121 are advertised in the device 106, when the part that contacts with batch of material melts A is platinum or platinum alloy, because oxygen can react with platinum or platinum alloy and produce PtO
2So, employed gas when advertising device 106 and advertise, preferred non-oxidizing gas with gas.As non-oxidizing gas, can enumerate oxygen partial pressure and be below 1%, preferred below 0.01%, the more preferably gas below 0.0001% preferred helium (He), neon (Ne), argon gas (Ar), krypton gas (Kr), xenon (Xe) or nitrogen (N
2) etc. neutral gas, perhaps carbon monoxide (CO) or hydrogen (H
2) wait reducing gas, perhaps be selected from the two or more mixed gas in the described gas.
In addition, air interchanger 110 is arranged on the top of melting furnace 102.This air interchanger 110 comprises: be formed with the conus portion 112 of suction port 114, the opening surface shape and the peristome 126 of this suction port 114 are roughly the same; And the vapor pipe 116 that connecting of conus portion 112 therewith.Moreover air interchanger 110 is examples that are used for discharging the air-releasing mechanism of the gas that is produced by the batch of material melts A in the fusion tank 121.
The discharge of the gas in the batch of material melting plant 100 is to use air interchanger 110, and the spatial volume during with melting furnace 102 fusions is a benchmark, (the batch of material fusion operation) of discharging with 2～20 times/minute speed.
And, in the air interchanger 110, the suction pump of one of utilization conduct attraction mechanism (suction device) example attracts the peristome with conus portion 112 opposite sides, (1hPa～1000hPa), the gas that exists in the superjacent air space with the batch of material melts A in the batch of material melting plant 100 is discharged simultaneously to be controlled to be 0.1kPa～100.0kPa with this air pressure with the fusion time space of batch of material melts A top.Further, in the present embodiment, have only a side (being the right side in the present embodiment) vapor pipe 116 extensions in the left and right sides and be connected to attraction mechanism, but as long as the air pressure of batch of material melts A top is controlled in the described scope, Zuo Ce vapor pipe also can extend and is connected to other fusing devices so.
Like this, pressure in the superjacent air space of batch of material melts A is controlled as and the roughly the same or subatmospheric suction side of normal atmosphere, and the gas that exists in the superjacent air space of the batch of material melts A in the fusion tank 121 is discharged towards the suction port 114 of air interchanger 110 from body of heater 122 inside via peristome 126 simultaneously.
In addition, as remaining gas in the batch of material melts A, having is that oxygen, the using gas of oxidizing gas advertised the gas that is blown into when device 106 is advertised, and more aerobic and platinum or platinum alloy react and the PtO that produces
2Deng.
Formal melting plant, formal fusion operation
Below, describe the formal melting plant that is used for making the good glass of the less and ageing-resistant phenomenon of platinum content, formal fusion operation in detail.
Shown in Fig. 1 (B) and Fig. 2 (B), the formal melting plant 200 that uses in the formal fusion operation comprises: melting furnace 202, be used for making the batch of material fusion to obtain formal melts, perhaps be used for making the glass cullet fusion that obtains in the glass cullet chemical industry preface to obtain formal melts D; Discharge the relief outlet 203 of formal melts D; Transfer lime 204 is as the path (conduit) of the formal melts D till from melting furnace 202 to subsequent handling; Gas is advertised device 206, advertises gas in described formal melts D; And, the gas in the superjacent air space of formal melts D is discharged as the routine air interchanger 210 of one of output mechanism.
Melting furnace 202 comprises: the fusion tank 221 of the container when becoming the glass cullet fusion; Cover the body of heater 222 that constitutes by heat-stable materials such as refractory brick around this fusion tank 221; And heating unit (not shown).
For fusion tank 221, consider the fusion, the required thermotolerance of clarification, erosion resistance of formal melts D and to factors such as the quality influence of formal melts D are less, preferably, at least the part that contacts with formal melts D for example is by the fusion tank quartzy, that platinum or platinum alloy constituted, the more preferably fusion tank that is made of platinum or platinum alloy.
Around the body of heater 222 covering fusion tanks 221, constituted by heat-stable materials such as refractory brick.On the top of this body of heater 222, formed in order in fusion tank 221, to drop into the peristome 226 of glass cullet.And this peristome 226 becomes in order to remaining gas in the formal melts D in the fusion tank 221 is imported to the inlet of suction port 214, and described suction port 214 is used for from the described survival gas of body of heater 222 inner discharges.
On transfer lime 204, be provided with not shown heating unit.Control the temperature of transfer lime 204 by this heating unit, thereby control the viscosity of the formal melts D in the transfer lime 204, and make the flow velocity of the formal melts D in the transfer lime 204 controlled.And as mentioned above, transfer lime 204 becomes the conduit of the formal melts D till (clarification operation, agitating procedure, slow cooling operation) from formal fusion operation to subsequent handling.
Gas is advertised device 206 and is inserted in the fusion tank 221 from described peristome 226.That is, the peristome double as gas that is used for advertising gas in melts is advertised the patchhole of device.For formal melts D is fully stirred, the structure that gas is advertised device 206 is the well-known structure that can produce larger bubbles as much as possible.For this gas is advertised device 206, consider their thermotolerance, to the erosion resistance of formal melts D and to factor such as the quality influence of formal melts D is less, preferably, for example the part that contacts with formal melts D at least is to advertise device by the gas that quartz, platinum or platinum alloy constitute, and particularly preferably is the gas that is made of platinum or platinum alloy and advertises device.
Employed gas when advertising device 206 with gas and advertise can at random be set.But, when the member or the gas of the formal melting plants 200 of formation such as fusion tank 221, transfer lime 204 are advertised in the device 206, when the part that contacts with formal melts D is platinum or platinum alloy, because oxygen can react with platinum or platinum alloy and produce PtO
2So, employed gas when advertising device 206 and advertise, preferred non-oxidizing gas with gas.As non-oxidizing gas, can enumerate oxygen partial pressure and be below 1%, preferred below 0.1%, the more preferably gas below 0.01% preferred helium (He), neon (Ne), argon gas (Ar), krypton gas (Kr), xenon (Xe) or nitrogen (N
2) etc. neutral gas, perhaps carbon monoxide (CO) or hydrogen (H
2) wait reducing gas, perhaps be selected from the two or more mixed gas in the described gas.
The discharge of the gas in the formal melting plant 200 is to use air interchanger 210, and the spatial volume during with melting furnace 202 fusions is a benchmark, (the formal fusion operation) of discharging with 2～20 times/minute speed.
And, in the air interchanger 210, the suction pump of one of utilization conduct attraction mechanism (suction device) example attracts the peristome with conus portion 212 opposite sides, (1hPa～1000hPa), the gas that exists in the superjacent air space with the formal melts D in the formal melting plant 200 is discharged simultaneously to be controlled to be 0.1kPa～100.0kPa with this air pressure with the fusion time space of formal melts D top.Further, in the present embodiment, have only a side (being the right side in the present embodiment) vapor pipe 216 extensions in the left and right sides and be connected to attraction mechanism, but as long as the spatial air pressure of formal melts D top is controlled in the described scope, Zuo Ce vapor pipe also can extend and is connected to other fusing devices so.
Like this, air pressure in the superjacent air space of formal melts D is controlled as and the roughly the same or subatmospheric suction side of normal atmosphere, and the gas that exists in the superjacent air space of the glass cullet melts D in the fusion tank 221 is discharged towards the suction port 214 of air interchanger 210 from body of heater 222 inside via peristome 226 simultaneously.
In addition, as remaining gas in the formal melts D, having is that oxygen, the using gas of oxidizing gas advertised the gas that is blown into when device 206 is advertised, and more aerobic and platinum or platinum alloy react and the PtO that produces
2Deng.
On transfer lime 204, be provided with not shown heating unit.Control the temperature of transfer lime 204 by this heating unit, thus the viscosity of the formal melts D in the control transfer lime 204, and its result makes that the flow velocity of the formal melts D in the transfer lime 204 is controlled.And as mentioned above, transfer lime 204 becomes the conduit of the formal melts D till (clarification operation, agitating procedure, slow cooling operation) from formal fusion operation to subsequent handling.
Moreover, in the present embodiment, gas is advertised device 106,206 and is inserted into fusion tank 121,221 respectively via the peristome 126,226 that is positioned at body of heater 122,222 tops, but be not limited thereto, for example, gas advertises that device 106,206 also can run through the side surface part of fusion tank 121,221 or bottom and gas is advertised in portion or bottom in batch of material melts A or formal melts D from the side.
Again, in the present embodiment, be in glass cullet chemical industry preface and these two fusion operations of formal fusion operation, using gas is advertised device 106,206 and is come advertising gas in batch of material melts A and the formal melts D respectively, but also can only advertise gas in any operation of glass cullet chemical industry preface or formal fusion operation.And, in not carrying out the operation that gas advertises, also can prepare to possess the stirrer of agitating wing, described agitating wing is used for stirring the melts (for example batch of material melts A or formal melts D) in the fusion tank (for example fusion tank 121 or fusion tank 221).The shape of this agitating wing is not particularly limited, and for example can use the agitating wing of well-known shapes such as spirrillum and formation.
And, in the present embodiment, in batch of material fusion operation and formal fusion operation, be provided with air-releasing mechanism, but also can in any operation, air-releasing mechanism be set.
In addition, in the present embodiment, just in formal fusion operation, be provided with air interchanger 210 in the set formal melting plant 200, but also can optionally omit air interchanger 210 as one of output mechanism example.And, also be provided as the air interchanger 110 of output mechanism in also can be in the glass cullet chemical industry preface set batch of material melting plant 100.In addition, when the air interchanger 110 that in batch of material melting plant 100, is provided with as output mechanism, also can optionally in formal melting plant 200, omit air interchanger 210.
As long as air interchanger 110 and 210 has the function of the gas discharge that exists in the superjacent air space that makes batch of material melts A, glass cullet melts D, can use well-known air interchanger with different shape and formation.
And, for transfer lime 204 grades that constitute formal melting plant 200, consider their thermotolerance, to the erosion resistance of glass and to factors such as the quality influence of formal melts D are less, preferably, at least be platinum or platinum alloy system in the part that contacts with formal melts D, but needn't be defined in these materials.
And, when the flow velocity of melts is situation such as to control by the parameter beyond the viscosity of melts, the pressure in for example fusion tank 221, heating unit (not shown) may not be set on transfer lime 204.
Described heating unit can use well-known heating unit, for example electricradiator, electric heater, heating power body, high-frequency induction heating apparatus or use heating unit that the burning of passing through gas etc. of burner etc. heats etc., further, transfer lime 204 preferably can heat by direct energising, but needn't be defined in this.
The manufacture method of opticglass
Then, use Fig. 2 (A) and Fig. 2 (B), the manufacture method of using described melting plant and manufacture method to make opticglass of the present invention is described.
At first, shown in Fig. 2 A, come, will be deployed into the SiO that contains more than 30%, below 70% in mass percent
2And/or 3% above, B below 20%
2O
3The batch of material that can make opticglass put in the fusion tank 121 of batch of material melting plant 100, and make its fusion.At this moment, using gas is advertised device 106, and non-oxidizing gas is blasted in the batch of material melts A that makes frit fusion (thick fusion) and obtain.This gas is advertised in the following way and is carried out: the degree of depth place more than the liquid level 100mm of the batch of material melts A in distance fusion tank 121, at the volume of per 1 liter of batch of material melts A, be blown into non-oxidizing gas (glass cullet chemical industry preface) with 0.002～0.05 liter/minute feed speed.The batch of material melts A that obtained of casting outside stove, and reclaim as glass cullet.
Then, shown in Fig. 2 (B), the glass cullet that reclaim are put in the fusion tank 221 of formal melting plant 200, and made its fusion.At this moment, using gas is advertised device 206, and non-oxidizing gas (for example argon gas) is blasted in the formal melts D that makes glass cullet fusion (formal fusion) and obtain.This gas is advertised in the following way and carried out: the degree of depth place more than the liquid level 100mm of the formal melts D in distance fusion tank 221 at the volume of per 1 liter of formal melts D, is blown into non-oxidizing gas with 0.002～0.05 liter/minute feed speed.
And, in making glass cullet fused operation, utilize as the suction pump that attracts one of mechanism's (suction device) example to attract, and the gas of formal melts D top is discharged (formally fusing operation) from air interchanger 210.At this moment, (1hPa～1000hPa), the gas of then formal melts D top can be discharged well if the control suction pump is made as 0.1kPa～100.0kPa with the air pressure with formal melts D top.And, be benchmark preferably with the fusion time space volumes in the melting furnace 202, replace gas in the formal melting plant 200 with 2～20 times/minute speed.From then on the formal melts D that is obtained formally fuses operation and transfers to subsequent handling (clarification operation, agitating procedure, cold insulation operation), makes opticglass in subsequent handling.
In addition, in the present embodiment, in the raw materials melt operation, make after the frit fusion, make its quenching and make the solidified glass cullet, and the glass cullet of manufacturing are put in the fusion tank 221 and obtain formal melts D, and then continuously melts is supplied to subsequent handling, but formal fusion operation also can be to carry out in the batch of material mode, but not continuous mode.
Below, use embodiment and comparative example that the present invention is described in further detail, but the present invention is not limited to following embodiment.
Embodiment
With the opticglass that utilizes manufacture method of the present invention and make opticglass as embodiment, and the opticglass opticglass as a comparative example that will utilize other method and make, to the i line (365nm) of these glass irradiation ultrahigh pressure mercury lamps, the variation of measuring the transmissivity of this moment.
Embodiment 1
Come weighing opticglass raw material (frit) according to the proportion of composing shown in the table 1, and they are mixed.
Table 1
| No. | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example |
| SiO 2 | 63 | 60 | 60 | 60 | 58 | 51 | 60 |
| B 2O 3 | 8 | 15 | 11 | 6 | 10 | 17 | 15 |
| Al 2O 3 | 1 | 0 | 0 | 0 | 2 | 0 | 0 |
| K 2O | 20 | 15 | 18 | 14 | 6 | 10 | 15 |
| F | 8 | 10 | 5 | 0 | 0 | 0 | 10 |
| |
0 | 0 | 3 | 10 | 15 | 10 | 0 |
| |
0 | 0 | 1 | 1 | 0 | 0 | 0 |
| Li 2O | 0 | 0 | 0 | 1 | 0 | 0 | 0 |
| Na 2O | 0 | 0 | 1 | 1 | 5 | 7 | 0 |
| |
0 | 0 | 1 | 7 | 3 | 5 | 0 |
| As 2O 3 | 0.1 | 0.01 | 0.01 | 0.01 | 0.01 | 0.01 | 0 |
| Sb 2O 3 | 0 | 0 | 0 | 0 | 0 | 0 | 0.01 |
| Add up to | 100.1 | 100.01 | 100.01 | 100.01 | 99.01 | 100.01 | 100.01 |
| Advertise | Ar | Ar | Ar | Ar | Ar | Ar | O 2 |
| Pt measures (ppm) | 0.10 | 0.12 | 0.14 | 0.21 | 0.26 | 0.29 | 0.70 |
| Transition metal amount (ppm) | 2.6 | 2.4 | 2.3 | 2.9 | 2.5 | 2.8 | 3.1 |
| Transmissivity deterioration rate (%) (500hr irradiation) | -0.098 | -0.084 | -0.100 | -0.110 | -0.138 | -0.157 | -0.214 |
Subsequently, frit is put in the fusion tank 121 of batch of material melting plant 100,1300 ℃ of glass cullet chemical industry prefaces of carrying out 14 hours.At this moment, do not carry out gas and advertise,, reclaim as glass cullet with the cooling of batch of material melts.The glass cullet of this recovery are put in the fusion tank 221 of formal melting plant 200,1150 ℃ of fusions of carrying out 15 hours.At this moment, using gas is advertised device 206, advertises argon gas in the formal melts D that glass cullet fusion (formal fusion) is obtained.This advertises is with 0.024 liter/minute gas feed speed, with advertising of carrying out apart from the degree of depth of the liquid level 500mm that advertises to per 1 liter of glass.In addition, in this fusion operation, the space of formal melts D top compared with normal atmosphere be made as decompression state (air pressure of the superjacent air space of formal melts D is 0.3kPa), the gas that exists in the superjacent air space with formal melts D is sucked by air interchanger 210 thus, and is discharged to (formal fusion operation) in the atmosphere.The formal melts D that is obtained is transferred to subsequent handling (clarification operation, agitating procedure, cold insulation operation), make the opticglass of present embodiment.
Comparative example
Come the frit of the opticglass of this comparative example of weighing according to the proportion of composing identical, and they are mixed with embodiment 1.Subsequently, this frit is put in the fusion tank 121 of raw materials melt device 100,1300 ℃ of glass cullet chemical industry prefaces of carrying out 14 hours.At this moment, do not carry out gas and advertise,, reclaim as glass cullet with the cooling of batch of material melts.The glass cullet of this recovery are put in the fusion tank 221 of formal melting plant 200,1150 ℃ of fusions of carrying out 15 hours.At this moment, using gas is advertised device 206, advertises " oxygen " in the formal melts D that glass cullet fusion (formal fusion) is obtained.This advertises is with 0.024 liter/minute gas feed speed, with advertising of carrying out apart from the degree of depth of the liquid level 500mm that advertises to per 1 liter of glass.In addition, in making this glass block fused operation, do not discharge gas (formal fusion operation) from the superjacent air space of formal melts D.The formal melts D that is obtained is transferred to subsequent handling (clarification operation, agitating procedure, cold insulation operation), make the opticglass of this comparative example.
Then, with 2.5W/cm
2Condition, to the opticglass irradiation i line (365nm) of the opticglass of embodiment and comparative example, the variation of measuring the transmissivity of this moment.In addition, transmissivity is to utilize U-4000 (Hitachi's manufacturing) and the transmissivity of the light of the wavelength 365nm that measures.
The variation of the transmissivity of Fig. 3 when to be expression to the opticglass of the opticglass of embodiment and comparative example shine i line (365nm).As shown in Figure 3, soon, the deterioration rate of the transmissivity of the opticglass of comparative example is just greater than the opticglass of embodiment after the irradiation.And along with the passing of irradiation time, it is apparent that this tendency becomes.So, by air line being set with the gas in the superjacent air space of discharging the glass cullet melts, and using gas advertises device advertise gas in batch of material melts and/or formal melts, and the opticglass of ageing resistance excellence can be provided.
And the deterioration amount and the Pt content of the composition of the opticglass of embodiments of the invention, the transmissivity under i line irradiation (500 hours) are as shown in table 1.
As shown in Table 1, the Pt content of embodiment 1 to 6 is compared less with the Pt content of comparative example, the ageing resistance excellence.
Claims (18)
1, a kind of opticglass, it contains SiO
2And/or B
2O
3, this opticglass is characterised in that,
Pt content (quality criteria) wherein is below the 5ppm.
2, opticglass according to claim 1 is characterized in that,
Come in mass percent, described opticglass contains the SiO more than 30%, below 70%
2And/or 3% above, B below 20%
2O
3
3, opticglass according to claim 1 and 2 is characterized in that,
Come in mass percent, described opticglass contains following compositions:
(a) SiO
2: 30～70% and/or
B
2O
3: 3～20% and/or
PbO:0～2% and/or
Al
2O
3: 0～6% and/or
Li
2O:0～5% and/or
CaO:0～2% and/or
TiO
2: 0～0.5% and/or
As
2O
3: 0～1% and/or
Sb
2O
3: 0～1% and/or
Na
2O:0～13% and/or
K
2O:0～23% and/or
BaO:0～42% and/or
ZnO：0～7％
And
(b) the total amount of part or all of described oxide compound F in the fluorochemical of displacement gained is 0～11%.
4, according to the described opticglass of arbitrary claim in the claim 1 to 3, it is characterized in that,
Come Na in mass percent
2O+K
2O+BaO+ZnO is 10～45%.
5, according to the described opticglass of arbitrary claim in the claim 1 to 4, it is characterized in that,
Come in mass percent, SrO is 0～2% and/or ZrO
2Be 0～2%.
6, according to the described opticglass of arbitrary claim in the claim 1 to 5, it is characterized in that,
Come CaO+SrO+ZrO in mass percent
2Be 0～2%.
7, according to the described opticglass of arbitrary claim in the claim 1 to 6, it is characterized in that,
Come in mass percent, described opticglass contains 50.5～70% described SiO
2, 3～15% described B
2O
3, the described Al below 2.9%
2O
3And the described Li below 4.9%
2O.
8, according to the described opticglass of arbitrary claim in the claim 1 to 7, it is characterized in that,
Come in mass percent, described opticglass contains 55.35～70% described SiO
2, the described A1 below 2.3%
2O
3And the described Li below 3%
2O.
9, according to the described opticglass of arbitrary claim in the claim 1 to 8, it is characterized in that,
The total content (quality criteria) of V, Cr, Mn, Fe, Co, Ni, Cu, Ag, W, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Dy, Ho, Fr, Tm, Yb, each composition of Lu is below the 3ppm.
10, a kind of manufacture method of opticglass, it comprises following operation: " with raw mix (below be called batch of material) fusion and obtain the operation (below be called glass cullet chemical industry preface) of glass cullet " and/or " with glass cullet and/or batch of material fusion and obtain the operation (below be called formal fusion operation) of glass ", the manufacture method of described opticglass is characterised in that
Contain SiO in the composition of the glass that is obtained
2And/or B
2O
3, and
In the melts of described glass cullet chemical industry preface and/or described formal fusion operation, advertise non-oxidizing gas.
11, the manufacture method of opticglass according to claim 10 is characterized in that,
Described non-oxidizing gas is blown into apart from the degree of depth more than the liquid level 100mm of described melts.
12, according to the manufacture method of claim 10 or 11 described opticglass, it is characterized in that,
Be blown into described non-oxidizing gas at per 1 liter of glass volume with 0.002～0.05 liter/minute feed speed.
13, according to the manufacture method of the described opticglass of arbitrary claim in the claim 10 to 12, it is characterized in that,
Described non-oxidizing gas is He, Ne, Ar, Kr, Xe, N
2, H
2, CO or these gases various mixed gases.
14, a kind of manufacture method of opticglass, it comprises following operation: will " raw mix (below be called batch of material) fusion and obtain the operation (below be called glass cullet chemical industry preface) of glass cullet " and/or " described glass cullet and/or batch of material fusion being obtained the operation (below be called formal fusion operation) of glass ", the manufacture method of described opticglass is characterised in that
Contain SiO in the composition of the glass that is obtained
2And/or B
2O
3System, and
Gas in the space in the melting plant in described glass cullet chemical industry preface and/or the described formal fusion operation is discharged.
15, the manufacture method of opticglass according to claim 14 is characterized in that,
In described glass cullet chemical industry preface and/or described formal fusion operation, make described batch of material and/or described glass cullet fusion, simultaneously the gas in the space in the described melting plant is discharged with it.
16, according to the manufacture method of claim 14 or 15 described opticglass, it is characterized in that,
With the spatial volume in the described melting plant is benchmark, replaces gas in this melting plant with 2～20 times/minute speed.
17, a kind of manufacturing installation of opticglass, described opticglass contains SiO at least
2And/or B
2O
3, the manufacturing installation of this opticglass is characterised in that,
Comprise: the batch of material fusion is obtained the batch of material melting plant of glass cullet and/or described glass cullet or described batch of material fusion are obtained the formal melting plant of glass melting thing, the non-oxidizing gas bubbling device is arranged in the described raw mix melting plant and/or in the described glass cullet melting plant.
18, a kind of manufacturing installation of opticglass, described opticglass contains SiO at least
2And/or B
2O
3, the manufacturing installation of this opticglass is characterised in that,
Comprise: fusion tank is used for making batch of material or glass cullet fusion and obtains melts; Body of heater, cover described fusion tank around, and have the peristome that drops into described batch of material or described glass cullet; And air-releasing mechanism, its configuration or connection are used for the gas that described melts produced in the described fusion tank is discharged near described peristome.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP317807/2005 | 2005-10-31 | ||
| JP317808/2005 | 2005-10-31 | ||
| JP317806/2005 | 2005-10-31 | ||
| JP2005317806A JP2007126296A (en) | 2005-10-31 | 2005-10-31 | Method and apparatus for manufacturing optical glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101296872A true CN101296872A (en) | 2008-10-29 |
Family
ID=38149258
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006800401496A Pending CN101296872A (en) | 2005-10-31 | 2006-10-23 | Optical glass, apparatus for producing optical glass, and process for producing the same |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP2007126296A (en) |
| CN (1) | CN101296872A (en) |
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Application publication date: 20081029 |