CN1915875B - Environmental protective heavy flint optical glass in high refractive index, and high dispersion, and producing method and equipment - Google Patents

Environmental protective heavy flint optical glass in high refractive index, and high dispersion, and producing method and equipment Download PDF

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Publication number
CN1915875B
CN1915875B CN2006100217220A CN200610021722A CN1915875B CN 1915875 B CN1915875 B CN 1915875B CN 2006100217220 A CN2006100217220 A CN 2006100217220A CN 200610021722 A CN200610021722 A CN 200610021722A CN 1915875 B CN1915875 B CN 1915875B
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opticglass
refractive index
glass
environmental protection
high refractive
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CN1915875A (en
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孙伟
陆明新
严从勋
刘家友
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CDGM Glass Co Ltd
Chengdu Guangming Optoelectronics Co Ltd
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Chengdu Guangming Optoelectronics Co Ltd
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Priority to CN2006100217220A priority Critical patent/CN1915875B/en
Priority to PCT/CN2006/002483 priority patent/WO2008028341A1/en
Priority to JP2008555598A priority patent/JP5044573B2/en
Publication of CN1915875A publication Critical patent/CN1915875A/en
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
    • C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
    • C03B5/18—Stirring devices; Homogenisation
    • C03B5/187—Stirring devices; Homogenisation with moving elements
    • 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
    • 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

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

Abstract

This invention provides a method for producing environmentally friendly heavy-flint optic glass with high refractivity and high color dispersion. The heavy-flint optic glass is composed of: SiO2 20-44 wt.%, TiO2 22-34 wt.%, Nb2O5 5-22 wt.%, Na2O 7-18 wt.%, BaO 9-17 wt.%, K2O 0-9 wt.%, CaO 0-3 wt.%, ZrO2 0-3 wt.%, SrO 0-0.5 wt.% and Sb2O3 0-0.5 wt.%. The method comprises (1) mixing the raw materials uniformly; (2) melting in a tank furnace at 1150-1300 deg.C to obtain glass liquid with uniform refractivity; (3) clearing, homogeneizing and molding the glass liquid into glass stripes; (4) annealing in an annealing furnace. The equipment comprises a tank furnace and an annealing furnace. The melting pool of the tank furnace is connected with an automatic burning control system. The heavy-flint optic glass dose not contains pollutive components such as PbO, As2O3 and GdO. The method can reduce the times of high-temperature melting and improve the optic permeability.

Description

The high chromatic dispersion environmental protection of high refractive index dense flint opticglass and preparation method and apparatus thereof
Technical field
The present invention relates to a kind of opticglass and preparation method and apparatus thereof, particularly relate to the high chromatic dispersion environmental protection of a kind of high refractive index (Nd) dense flint opticglass and preparation method and apparatus thereof.
Background technology
Raising along with people's living standard, in order to satisfy of the requirement of high-grade digital product height as number, small portable, the demand of dense flint opticglass with advantages such as high refractive index, high chromatic dispersion (low Abbe number), density are little is increasing, but the PbO that contains in the opticglass, As 2O 3With GdO environment is caused severe contamination, for this reason, optical device production firm requires to have in the glass of same optical properties and does not contain PbO, As 2O 3With the GdO composition.
In order to make opticglass have high refractive index, the TiO in the glass component 2And Nb 2O 5Corresponding also very big Deng the content of composition, glass metal viscosity is rare in the production process, crystallization serious because these components cause, the big and difficult forming of constant fluctuation, makes glass cord of low quality, and the production difficulty is very big.
Present opticglass manufacturer generally adopts tank furnace to produce in the mode of secondary material, production process is: the raw material for preparing at high temperature is fused into the suitable glass slag of granularity with single crucible behind thorough mixing, the specific refractory power of tested glass slag, the glass slag that specific refractory power is qualified is put in the high melt tank furnace again and is founded into glass metal, becomes the glass billot through clarification with abundant homogenizing aftershaping.Because this production method through twice high temperature, influenced the optical transmittance of glass, and operation is more, the production cycle is long, production cost is high.
Summary of the invention
Technical problem to be solved by this invention provides the high chromatic dispersion environmental protection of a kind of high refractive index dense flint opticglass, does not contain PbO, As in this opticglass component 2O 3And GdO.
The present invention also will provide a kind of production method of above-mentioned opticglass, and this method is only through a high temperature, and the optical transmittance of glass is good, and operation is few, and the cycle is short.
The present invention also will provide a kind of production unit of above-mentioned opticglass.
The technical scheme that technical solution problem of the present invention is adopted is: the high chromatic dispersion environmental protection of high refractive index dense flint opticglass, its weight percent consists of: SiO 2: 20-44%, TiO 2: 22-34%, Nb 2O 5: 5-22%, Na 2O:7-18%, BaO:9-17%, K 2O:0-9%, CaO:0-3%, ZrO 2: 1.1-3%, SrO:0-0.5%, Sb 2O 3: 0-0.5%.
The production method of the high chromatic dispersion environmental protection of high refractive index dense flint opticglass, this method may further comprise the steps: 1) with the raw material thorough mixing for preparing, guarantee its homogeneity; 2) under 1150-1300 ℃ high temperature, be fused into glass metal, make the specific refractory power consistence of glass metal good with tank furnace; 3) glass metal that specific refractory power is qualified is shaped to the glass billot through clarification with fully after the homogenizing; 4) the glass billot is annealed in annealing furnace.
The production unit of the high chromatic dispersion environmental protection of high refractive index dense flint opticglass comprises tank furnace and annealing furnace, and the molten pool of described tank furnace links to each other with automatic combustion control system.
The invention has the beneficial effects as follows: opticglass of the present invention does not contain PbO, As 2O 3With the component that GdO pollutes environment, its Nd is that 1.7-1.85, Vd (Abbe number) are 23.5-28.5, is the high chromatic dispersion environmental protection of high refractive index dense flint opticglass.The present invention adopts tank furnace to produce opticglass in the mode of once changing material, and Production Flow Chart is coherent, succinct, has reduced the high temperature melting number of times, under the identical condition of raw materials quality, can improve optical transmittance, and operation is few, with short production cycle, reduced production cost.
Description of drawings
Fig. 1 is the schema of the existing secondary material mode of production.
Fig. 2 is the schema that the present invention once changes the material mode of production.
Fig. 3 is the grid agitator synoptic diagram.
Fig. 4 is the disk stirrer synoptic diagram.(wherein: Fig. 4 a is the front view of disk stirrer; Fig. 4 b is the side-view of disk stirrer; Fig. 4 c is the attached view of the broken section of disk stirrer.)
Fig. 5 is a production unit synoptic diagram of the present invention.
Embodiment
The glass-former SiO that contains 20-44% in the opticglass of the present invention 2, if SiO 2Too high levels, then the specific refractory power of glass, chromatic dispersion index can not reach requirement, simultaneously glass melting temperature uprises, and is difficult for fusing; If SiO 2Content ratio low excessively, then can reduce crystal property and chemical stability, preferred SiO 2Content is 23-44%, particularly preferred SiO 2Content is 25-37%.
Except glass-former, also need a certain proportion of fusing assistant to be used for reducing the higher high refractive index component of glass melting temperature, the too high levels of fusing assistant then influences nonferromagnetic substance, the chemical stability of glass; The content of fusing assistant is low excessively, then high refractive index component infusibility.So fusing assistant Na in the glass 2O+K 2The total content of O is 7-27%, wherein Na 2The content of O is 7-18%, K 2The content of O is 0-9%; Preferred Na 2The content of O is 10-16%, K 2The content of O is 0-8%; Particularly preferred Na 2The content of O is 12-15%, K 2The content of O is 0-8%
For the optical index that makes glass reaches requirement, must contain the component of the high refractive index of higher proportion, so glass-former SiO 2With fusing assistant Na 2O and K 2The ratio of O just is restricted, preferred SiO 2+ Na 2O+K 2The total content of O is no more than 50%, particularly preferred SiO 2+ Na 2O+K 2The total content of O is no more than 45%.
Alkaline earth metal oxide BaO, CaO and SrO can adjust the microtexture of glass, improve the chemical stability of glass, and the total content of preferred BaO+CaO+SrO is 10-20%, wherein, the content of BaO is 9-17%, and the content of CaO is 0-3%, and the content of SrO is 0-0.5%; The total content of particularly preferred BaO+CaO+SrO is 12-18%, and wherein the content of BaO is 12-16%, and the content of CaO is 0-3%, and the content of SrO is 0-0.5%.
TiO 2Can make glass have high refractive index, but too high levels can reduce abbe number greatly and increase tendency towards devitrification greatly; Content is too small can't to meet the requirements of high refractive index again, so TiO 2Content is 22-34%, preferred 27-34%, particularly preferred 28-32%.
Nb 2O 5Can make glass have high refractive index, with an amount of Nb 2O 5Substitute TiO 2Can guarantee that glass has high refractive index, reduce tendency towards devitrification simultaneously, but too much Nb 2O 5Content can make specific refractory power, abbe number can not reach requirement so Nb simultaneously 2O 5Content is 5-22%, preferred 10-22%, preferred especially 12-20%.
ZrO 2Can make glass have high refractive index, improve glass chemistry stability, expansion character simultaneously, can use ZrO 2The alternative TiO of part 2, make the photosensitiveness index reach requirement, but ZrO 2Too high levels can increase tendency towards devitrification, reduce specific refractory power, so ZrO 2Content is 1.1-3%, preferred 1.1-2%, preferred especially 1.1-1.5%.
Sb 2O 3Be finings, can and emit gas with other gas generation reversible absorption, small gas is accumulated into than atmospheric, in glass metal, eliminate by floating to the back, surface on the buoyancy in the differing temps district in glass smelting stage, but Sb 2O 3The work-ing life that content too much can influence glass colourity and reduce the platinum container, so Sb 2O 3Content is 0-0.5%, preferred 0-0.3%, preferred especially 0-0.15%.
Table 1 is 9 embodiment of opticglass of the present invention.
1 2 3 4 5 6 7 8 9
SiO 2 22.9 24.0 26.0 27.0 34.0 37.0 38.0 41.0 42.1
TiO 2 29.1 28.0 30.0 28.0 28.0 25.0 28.0 27.0 25.9
Nb 2O 5 19.0 19.0 14.0 13.0 11.0 10.0 9.6 8.0 8.0
Na 2O 12.0 12.0 13.0 9.0 12.0 14.0 14.0 15.0 15.0
BaO 16.0 16.0 15.0 13.0 12.0 14.0 10.0 9.0 9.0
K 2O 0 0 0 7.5 3 0 0 0 0
CaO 0 0 0.1 2 0 0 0 0 0
ZrO 2 0 1.1 2.0 0 0 0 0 0 0
SrO 0.3 0.3 0 0 0 0 0 0 0
Sb 2O 3 0.03 0.03 0.03 0.03 0.1 0.1 0.1 0.1 0.1
Nd 1.8535 1.8469 1.8452 1.8056 1.7852 1.7558 1.7620 1.7286 1.7210
Vd 23.62 23.77 23.85 25.51 25.80 27.60 26.58 28.40 28.46
Table 1
As can be seen from Table 1: opticglass of the present invention does not contain PbO, As 2O 3With the component that GdO pollutes environment, its photosensitiveness index is: Nd is that 1.7-1.85, Vd are 23.5-28.5.
Fig. 1 is the schema of the existing secondary material mode of production, and this production method comprises following a few step: batching; Fusion cast glass slag in single crucible; Check constant and group are criticized; Qualified glass slag is at tank furnace fusion cast glass liquid; Clarification; Homogenizing; Moulding; Annealing furnace annealing.
Fig. 2 is the schema that the present invention once changes the material mode of production, and the concrete steps of this production method are:
One: the raw material thorough mixing with preparing guarantees its homogeneity.
1) adopts quick moisture tester, strengthen the especially easily moisture monitoring of moisture absorption raw material of raw material, meet could using of opticglass raw material standard, defective forbidding; 2) batching adopts repeatedly weighing technique on a small quantity, and each weighing is not more than the powder of 30 kilograms of glass; Weighing equipment uses high precision weighing equipment (as electronic scales), and precision is 0.01kg; 3) adopt agitator to mix; 4) serious in order to prevent the raw material layering, adopt vanning on a small quantity, the glass powder of each vanning is no more than 30 kilograms; 5) owing to be that artificial timing is reinforced, be the layering that reduces transportation, deposits process, adopt manual the stirring before each the feeding in raw material again.
Two: under 1150-1300 ℃ high temperature, be fused into glass metal with tank furnace of the present invention, make the specific refractory power consistence of glass metal good.
1) bubbler of increase melting pool becomes 2-4 bubbler from 1; 2) adopt automatic combustion control system, keep the oxidizing atmosphere and the automatic attemperation of combustion flame, guarantee that temperature of fusion and atmosphere meet the stability of processing requirement; 3) increase the specific refractory power number of times of testing the melting pool glass metal, per 4 hours once, in time proofreaies and correct in case of necessity.Adopt the different homologous series glass trade mark of specific refractory power or raw material to proofread and correct, guarantee to proofread and correct and expect not introduce to be corrected the composition that does not have in the glass; 4) replace grid agitator with discoid agitator.Fig. 3 is the grid agitator synoptic diagram, and the stirring theory of grid agitator is to rely on frame 1 to stir and cut, and the width of frame 1 is less.Fig. 4 is the disk stirrer synoptic diagram, and disk 2 links together by axle, and frame 3 is arranged on the outward flange both sides of disk 2, and is stair shape and rises.The stirring theory of discoid agitator is the flow direction that changes glass metal by disk 2, and frame 3 cuts, and the width of frame 3 is bigger.Because glass viscosity is very little, very little to the agitator resistance that rotates, comparatively speaking the resistance that is subjected to of the discoid agitator that border width is bigger more greatly, stirring capacity is strong, can better stir sliminess glass.
Three: after the clarification of glass metal process and abundant homogenizing that specific refractory power is qualified, be shaped to the glass billot.
Four: the glass billot is annealed in annealing furnace.
The production method of once changing material is with respect to the advantage of the production method of secondary material: cancelled single crucible fusion cast glass slag link, the main purpose of this link is to guarantee glass metal specific refractory power consistence.The key that adopts tank furnace once to change the production method of material is, adopts an effective measure and guarantees the homogeneity of raw material to founding link from preparation raw material, and increase the consistence that supplementary unit improves the glass metal specific refractory power at fusion cast glass pendular ring joint.
Every technical indicator of the high chromatic dispersion environmental protection of the high refractive index that adopts production method of the present invention to produce dense flint opticglass all reaches technical target of the product, and optical transmittance is more excellent.With same raw material, adopt the H-ZF of the production method production of secondary material 52AColourity, interior all in the upper limit of OHARA standard, the H-ZF that adopts production method of the present invention to produce 52AColourity, interior all the lower limit of standard value (+10nm); With same raw material, adopt the H-ZF of the production method production of secondary material 7LABillot colourity, interior than the H-ZF that adopts production method of the present invention to produce 7LAColourity, the about 10nm of interior height, at the lower limit of standard value (10nm).
Production unit of the present invention as shown in Figure 5, comprise tank furnace and annealing furnace, the molten pool of tank furnace links to each other with automatic combustion control system, and wherein the annexation of automatic combustion control system is followed successively by: natural gas inlet mouth, filtration voltage-regulation voltage-stabilization automatic cut-off system, natural gas flow measurement Controlling System, ratio regulation system; Combustion air inlet mouth, voltage-regulation voltage-stabilization automatic cut-off system, combustion air flow measurement Controlling System, ratio regulation system; Wherein also have temperature controller between the melting pool of natural gas flow measurement Controlling System and tank furnace, described ratio regulation system is chewed with the burning of molten pool and is linked to each other.
Principle of work when production unit of the present invention is worked is: the ratio that configures natural gas and air on the ratio regulation system guarantees the abundant burning of natural gas, temperature controller measure tank furnace melting pool actual temperature value and contrast with set temperature value, send steering order and regulate the flow of natural gas to natural gas flow measurement Controlling System, the signal passing ratio regulation system of natural gas fluctuations in discharge is transferred to combustion air flow measurement Controlling System simultaneously, combustion air flow measurement Controlling System with the combustion air Flow-rate adjustment to being complementary with the natural gas flow, make the two flow reach set(ting)value, finally make temperature remain on design temperature, keep the stable of technology.

Claims (10)

1. the high chromatic dispersion environmental protection of high refractive index dense flint opticglass, it is characterized in that: its weight percent consists of: SiO 2: 20-44%, TiO 2: 22-34%, Nb 2O 5: 5-22%, Na 2O:7-18%, BaO:9-17%, K 2O:0-9%, CaO:0-3%, ZrO 2: 1.1-3%, SrO:0-0.5% and Sb 2O 3: 0-0.5%.
2. the high chromatic dispersion environmental protection of high refractive index as claimed in claim 1 dense flint opticglass is characterized in that: described SiO 2, Na 2O and K 2Weight percent sum≤50% of O, the weight percent sum of BaO, CaO and SrO is 10-20%.
3. the high chromatic dispersion environmental protection of high refractive index as claimed in claim 1 dense flint opticglass, it is characterized in that: its weight percent consists of: SiO 2: 23-44%, TiO 2: 27-34%, Nb 2O 5: 10-22%, Na 2O:10-16%, BaO:12-16%, K 2O:0-8%; CaO:0-3%, ZrO 2: 1.1-2%, SrO:0-0.5% and Sb 2O 3: 0-0.3%.
4. the high chromatic dispersion environmental protection of high refractive index as claimed in claim 1 dense flint opticglass, it is characterized in that: its weight percent consists of: SiO 2: 25-37%, TiO 2, 28-32%, Nb 2O 5: 12-20%, Na 2O:12-15%, BaO:12-16%, K 2O:0-8%, CaO:0-3%, ZrO 2: 1.1-1.5%, SrO:0-0.5% and Sb 2O 3: 0-0.15%.
5. the high chromatic dispersion environmental protection of high refractive index as claimed in claim 4 dense flint opticglass is characterized in that: described SiO 2, Na 2O and K 2Weight percent sum≤45% of O, the weight percent sum of described BaO, CaO and SrO is 12-18%.
6. the production method of the high chromatic dispersion environmental protection of the described high refractive index of claim 1 dense flint opticglass, it is characterized in that: this method may further comprise the steps: 1) with the raw material thorough mixing for preparing, guarantee its homogeneity; 2) under 1150-1300 ℃ high temperature, be fused into glass metal, make the specific refractory power consistence of glass metal good with tank furnace; 3) glass metal that specific refractory power is qualified is shaped to the glass billot through clarification with fully after the homogenizing; 4) the glass billot is annealed in annealing furnace.
7. the production method of the high chromatic dispersion environmental protection of high refractive index as claimed in claim 6 dense flint opticglass, it is characterized in that: when carrying out described step 1, adopt quick moisture tester that the opticglass raw material is carried out the moisture monitoring, meet could using of opticglass raw material standard, defective forbidding.
8. the production unit of the high chromatic dispersion environmental protection of the described high refractive index of claim 1 dense flint opticglass comprises tank furnace and annealing furnace, and it is characterized in that: the molten pool of described tank furnace links to each other with automatic combustion control system.
9. the production unit of the high chromatic dispersion environmental protection of high refractivity as claimed in claim 8 dense flint opticglass, it is characterized in that: the annexation of described automatic combustion control system is followed successively by: natural gas inlet mouth, filtration voltage-regulation voltage-stabilization automatic cut-off system, natural gas flow measurement Controlling System, ratio regulation system; Combustion air inlet mouth, pressure regulation, voltage stabilizing, automatic cut-off system, combustion air flow measurement Controlling System, ratio regulation system; Wherein also has temperature controller between the melting pool of natural gas flow measurement Controlling System and tank furnace; Described ratio regulation system is chewed with the burning of molten pool and is linked to each other.
10. the production unit of the high chromatic dispersion environmental protection of high refractive index as claimed in claim 8 dense flint opticglass, it is characterized in that: the agitator of described tank furnace adopts discoid agitator, disk (2) links together by axle, and frame (3) is arranged on the outward flange both sides of disk (2).
CN2006100217220A 2006-08-31 2006-08-31 Environmental protective heavy flint optical glass in high refractive index, and high dispersion, and producing method and equipment Active CN1915875B (en)

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CN2006100217220A CN1915875B (en) 2006-08-31 2006-08-31 Environmental protective heavy flint optical glass in high refractive index, and high dispersion, and producing method and equipment
PCT/CN2006/002483 WO2008028341A1 (en) 2006-08-31 2006-09-21 Environmental protection type dense flint glass with high refractive index and high dispersion, and method and device for preparing the same
JP2008555598A JP5044573B2 (en) 2006-08-31 2006-09-21 High refractive index, high dispersibility environmental countermeasure heavy flint optical glass and manufacturing method and equipment

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CN1915875B true CN1915875B (en) 2010-08-18

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
US9988296B2 (en) 2016-09-05 2018-06-05 Cdgm Glass Co., Ltd. Optical glass and optical element

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