CN102351419A - K9 optical glass and preparation method thereof - Google Patents
K9 optical glass and preparation method thereof Download PDFInfo
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- CN102351419A CN102351419A CN2011101832406A CN201110183240A CN102351419A CN 102351419 A CN102351419 A CN 102351419A CN 2011101832406 A CN2011101832406 A CN 2011101832406A CN 201110183240 A CN201110183240 A CN 201110183240A CN 102351419 A CN102351419 A CN 102351419A
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Abstract
The invention relates to a K9 optical glass. The K9 optical glass comprises the following components, by weight, 66-71% of SiO2, 1-2% of BaO, 6-9% of K2O, 5-8% of Na2O, 1-2% of ZnO, 8-11% of B2O3, 1-2% of CaO, and 0.2-0.6% of Sb2O3. The invention also relates to a preparation method of the K9 optical glass. The preparation method comprises the following steps: 1, fully melting materials in a melting pool, and allowing the materials to enter a clarification pool, wherein the materials comprise clinkers and raw materials; 2, clarifying a liquid glass in the clarification pool to eliminate bubbles in the liquid glass; 3, allowing the liquid glass to enter a platinum work pool, and stirring the liquid glass with a platinum stirrer; and 4, allowing the liquid glass to flow out through a platinum discharge tube to obtain the K9 optical glass. According to the K9 optical glass and the preparation method thereof in the invention, Sb2O3 is adopted as a clarificant to replace severely toxic As2O3, so the pollution of the poisonous and harmful substance As2O3 is avoided; K2O is introduced by K2CO3, so pollutive gases of NO and NO2 generated by KNO3 decomposition are avoided; and Na2CO3 is adopted to replace Na2SO4, so SO3 generated in Na2SO4 decomposition is avoided.
Description
Technical field
The invention belongs to the opticglass field, be specifically related to a kind of K9 opticglass and preparation method thereof.
Background technology
K9 opticglass mainly is used as lens and the prism in the optical system, is used for the transmission of picture, is the core of opticinstrument.
The composition (WT%) of tradition K9 opticglass
There is following problem in above-mentioned traditional K9 opticglass:
1, AS in the prescription
2O
3Be hazardous and noxious substances, environment is had pollution.
2, glass is in melting process, because adopted KNO
3So, can form NO, NO
2Dusty gas.
Summary of the invention
Technical problem to be solved by this invention provides a kind of K9 opticglass and preparation method thereof, through change component composition, and manufacturing process, change the generation of obnoxious flavour in traditional K9 opticglass production, improve the opticglass quality of production.
For solving the problems of the technologies described above, the technical scheme that the present invention takes is: a kind of K9 opticglass, and the weight ratio WT% of product component is:
SiO2：66-71；
BaO：1-2；
K2O：6-9；
Na2O：5-8；
ZnO：1-2；
B2O3：8-11；
CaO：1-2；
Sb2O3：0.2-0.6。
A kind of method for preparing K9 opticglass is made up of following steps:
Step 1: raw material is mixed by grog and raw material and forms, and raw material is fully fusing in melting pool, and the material road gets into settling pond through rising;
Step 2: liquid glass is clarified in settling pond, eliminates the inner bubble of glass;
Step 3: liquid glass gets into the platinum work pool, adopts platinum agitator liquid towards glass to stir;
Step 4: liquid glass flows out through the platinum discharge nozzle, obtains K9 opticglass.
Melting pool adopts three-phase alternating current to the raw material direct heating in the said step 1.
Melting pool top is provided with the raw material layer in the said step 1, when reinforced, feeds in raw material through liquid level appearance monitoring level fluctuation amplitude.
Raw material and grog add in the 4:1 ratio in the reinforced process of said step 1, add raw material earlier, add grog again.
Settling pond adds finings in the said step 2, and finings adopts Sb2O3.
Said raw material are by SiO
2, BaCO
3, KCO
3, Na
2CO
3, ZnO, H
3BO
3, CaCO
3, Sb
2O
3Form, said grog is the product of raw material gained after step 1-4 processing.
A kind of K9 opticglass of the present invention and preparation method thereof, coefficient of expansion α: 69 * 10
-7/ ℃≤α≤89 * 10
-7/ ℃, specific refractory power is 1.510～1.520, and high temperature viscosity is little, is suitable for the tank furnace continuous production.
Melting pool adopts three-phase alternating current can farthest accomplish the alternating current phases balance, and adopts joule heating that frit is heated, and accomplishes maximum energy utilization rate.
In the opticglass production process, the amount of increase and amount of decrease of glass liquid level can produce bigger influence to product quality, and the liquid level appearance can be monitored the ups and downs of glass liquid level well, and the control accuracy of liquid level appearance is in ± 1mm.
Because adopt cold top technology, melting pool top is provided with certain thickness raw material layer, the raw material layer has completely cut off the melting end great amount of heat, has promptly reduced also save energy of charge temperature.When reinforced, feed in raw material according to the height change of liquid level, level fluctuation is controlled at ± 1mm.Raw material and grog ratio add in the ratio of 4:1, add raw material earlier, add grog again; Help the abundant fusing of raw material.
Finings Sb
2O
3Decomposition reaction be reversible reaction, the reversible reaction temperature is about 1220 ℃.Sb during high temperature
2O
3Decompose O
2, absorb O during low temperature
2Sb in settling pond
2O
3Decompose O
2, the bubble that glass is contained is grown up, emersion glass; Sb behind the settling pond
2O
3Absorb O
2, make glass inside contain O
2Bubble reduce, finally absorbed by glass, reach the purpose of eliminating bubble.
A kind of K9 opticglass of the present invention and preparation method thereof adopts Sb
2O
3Substitute the AS of severe toxicity
2O
3As finings, stopped AS
2O
3The pollution of venomous injurant; K
2O is with K
2CO
3Form is introduced, and has stopped KNO
3Decompose the NO, the NO that are produced
2Dusty gas; Adopt Na
2CO
3Replace Na
2SO
4, stopped Na
2SO
4The SO that produces during decomposition
3
Embodiment
Embodiment 1: a kind of K9 opticglass, and the weight ratio WT% of product component is:
SiO
2：68.6；
BaO：1.3；
K
2O：8.2；
Na
2O：7.6；
ZnO：1.5；
B
2O
3：10.5；
CaO：1.8；
Sb
2O
3：0.5。
Embodiment 2: a kind of K9 opticglass, and the weight ratio WT% of product component is:
SiO
2：67.8；
BaO：1.7；
K
2O：8.8；
Na
2O：7.4；
ZnO：1.8；
B
2O
3：10.2；
CaO：1.9；
Sb
2O
3：0.4。
Embodiment 3: a kind of K9 opticglass, and the weight ratio WT% of product component is:
SiO
2：69.9
BaO：1.3
K
2O：8.4
Na
2O：7.5
ZnO：1.2
B
2O
3：10.3
CaO：1.1
Sb
2O
3：0.3。
The straight smelting technology of the cold roof pendant of all-electric melting is adopted in the kiln design, has reduced the volatilization of product component, and product homogeneity and the consistence produced are fully controlled.
Raw material is fully fusing in melting pool, and the material road gets into settling pond through rising; Glass is clarified in settling pond, eliminates the inner bubble of glass; Get into a special platinum work pool again, adopt the platinum agitator that glass is stirred, platinum work pool and platinum agitator can be reduced to minimum level with pollution as far as possible, and glass is abundant homogenizing in the platinum work pool, obtains the uniform product of component height; Flow out through the platinum discharge nozzle again,, finally obtain satisfactory K9 opticglass product through the forming mould moulding of different size.
Melting pool adopts three-phase alternating current that raw material is carried out direct heating, heater voltage 380V (± 1V), the about 1500A of electric current (± 0.1A).
For obtaining optics K9 glass of the present invention, the present invention adopts following specific installation:
A, Ingredient Production Line:
Optics K9 is high to the uniformity coefficient requirement of glass ingredient, and the present invention adopts mixture homogeneity to prepare burden greater than 98% Ingredient Production Line, to obtain the raw material of high evenness.
B, quick anneal oven:
Optical glass refractive index and Abbe number index are directly proportional with the logarithm of glass annealing speed.Glass sample detects its specific refractory power with certain speed annealing back and Abbe number is the important means of control product specific refractory power and Abbe number.Through quick anneal oven glass sample speed is on demand annealed.
C, high precision V prism:
For accurately controlling the opticglass leading indicator: specific refractory power and Abbe number, the detection in the production process is particularly important, generally is the sample behind the short annealing furnace annealing is detected.High precision V prism is the visual plant that detects specific refractory power and Abbe number in the production process.
D, liquid level appearance:
In the opticglass production process, the ups and downs of glass liquid level can produce bigger influence to product quality.The liquid level appearance can be monitored the ups and downs of glass liquid level well, and the control accuracy of liquid level appearance requires in ± 1mm.
E, bridge-type stirrer:
Bridge-type stirs the central position and the height of the accurate platinum stirring rod easily of function, to obtain the product of high uniformity.
F, up-down shaper:
The shape and the specification of the finished product are controlled by forming mould, and forming mould is installed on the shaper.The up-down shaper can be adjusted product thickness easily, changes specification fast, satisfies client's different demands.
G, netted belt-conveyor furnace:
Glass temperature after the shaper moulding is than higher, and directly cooling can cause product to burst.Lower the temperature with certain speed through netted belt-conveyor furnace, product stress is reduced, avoided bursting of product; Simultaneously can satisfy the common customer requirement.
H, schlieren instrument:
Opticglass is had relatively high expectations to the striped of glass inside as the element of optical imagery; The bad meeting of striped directly influences the quality of optical imagery.Schlieren instrument passes through the detection to sample, directly the quality of the inner striped of qualitative detection glass.
I, spectrophotometer:
Spectrophotometer is used for the test products transmitance.J, fine annealing stove:
The fine annealing stove can be adjusted to the data that the client needs with product stress and specific refractory power according to client's demand.
K, stressometer:
Through stressometer quantitative test glass strain.
Opticglass is high to ingredient requirement, must detect raw material before the batching, mainly contains following equipment: electronic balance, constant temperature oven.
Opticglass production requires must reach more than 98% to the raw material uniformity coefficient, for reaching above uniformity coefficient, takes following operation steps:
1., all raw material pile up separately, avoid between the raw material polluting mutually.Raw material is mixed by grog and raw material and forms.
Raw material are by SiO
2, BaCO
3, KCO
3, Na
2CO
3, ZnO, H
3BO
3, CaCO
3, Sb
2O
3Form, said grog is the bulk product of raw material gained after processing.
2., weight percent adopts the electronic scales weighing of precision 0.01Kg in the component greater than 1% raw material; Weight percent adopts the electronic scales weighing of precision 0.5g in the component less than 1% raw material.
3., the weighing order is carried out weighing by the principle of small powder after the first aniseed.
4., mixer adopts the V-type mixer, the batch mixing uniformity coefficient reaches more than 98%.
5., charge temperature, method, give birth to the grog ratio.
Owing to adopt cold top technology, the raw material layer about the about 150mm in melting pool top.Charge temperature is below 100 ℃; About 1200 ℃ of temperature of fusion; About 1380 ℃ of clarifying temps.
When reinforced, feed in raw material according to the height change of liquid level, level fluctuation is controlled at ± 1mm.Raw material and grog ratio add in the ratio of 4:1, add raw material earlier, add grog again.
Stokehold optical constant mensuration, correction parameter, bearing calibration:
The stokehold optical constant is measured:
Short annealing furnace temperature be raised to annealing temperature insulation, put into quick anneal oven in the settling pond sampling then, by-250 ℃/H annealing 1., earlier;
2., the appearance after will annealing is processed into 20*20*10, the samples of two right angle face correct grindings;
3., with the optical constant of V prism specimen.
Carry out the setting of stokehold data based on the requirement of counter stress, concrete data are the standard value fire increment of going down.The data that the sample data that tests out and stokehold are set compare, and exceed the deviation of processing requirement like deviation, then carry out the stokehold and proofread and correct, the concrete correction as follows:
Nd is higher than standard 50*10
-5, use SiO
2Proofread and correct, per kilogram reduces 4.7*10
-5
Nd is higher than standard 50*10
-5, proofread and correct per kilogram rising 22*10 with BaO
-5
Adopt SiO
2With the BaO timing, in advance with correction material with cooperate powder by the 1:1 mixed after add.
Glass gets into settling pond after heating up through uptake, and glass temperature reaches about 1380 ℃ in the settling pond, and settling time is about 40 minutes.The process that bubble is eliminated has dual mode:
1., bubble in the process that temperature rises, with the rising of temperature, the volume of bubble strengthens, buoyancy that bubble rises and lift velocity also increase simultaneously; Simultaneously, with the rising of temperature, glass viscosity also reduces, and the resistance that bubble is risen reduces, and the speed that bubble is risen increases.
2., the effect of finings:
Sb
2O
3Decomposition reaction be reversible reaction, the reversible reaction temperature is about 1220 ℃.Sb during high temperature
2O
3Decompose O
2, absorb O during low temperature
2Sb in settling pond
2O
3Decompose O
2, the bubble that glass is contained is grown up, emersion glass; Sb behind the settling pond
2O
3Absorb O
2, make glass inside contain O
2Bubble reduce, finally absorbed by glass, reach the purpose of eliminating bubble.
The agitator installation site is blade pitch work pool bottom 10-20mm, apart from work pool side 10 mm of portion; The agitator revolution generally is set at 40 rev/mins, suitably increases and decreases according to the striped situation; Glass is 30 minutes in the work pool residence time; With the rotation of agitator, glass seethes in work pool, is stirred the device blade cuts simultaneously, makes its component full and uniform, eliminates its striped.
Glass is eliminated bubble through clarification, through the work pool agitator stir eliminate striped after, flow out moulding by the platinum discharge nozzle of particular design with certain load.The specification of moulding is by the speed control of forming mould and netted belt-conveyor furnace.The certain situation compacted under width of load is controlled by the forming mould width; Thickness is by the netted belt-conveyor furnace speed control.The control of load is controlled each section of discharge nozzle temperature control automatically by the high precision silicon controlled rectifier, and under the temperature-resistant situation of each section of discharge nozzle, it is constant that load will keep.General mold temperature is about 950 ℃.
According to glass property, its softening temperature is 545 ℃, and setting the fine annealing temperature is 520 ℃.The set basis of annealing curve requires the requirement of counter stress and data to set.
Claims (7)
1. a K9 opticglass is characterized in that, the weight ratio WT% of product component is:
SiO
2：66-71；
BaO：1-2；
K
2O：6-9；
Na
2O：5-8；
ZnO：1-2；
B
2O
3：8-11；
CaO：1-2；
Sb
2O
3：0.2-0.6。
2. method for preparing the described K9 opticglass of claim 1 is characterized in that being made up of following steps:
Step 1: raw material is mixed by grog and raw material and forms, and raw material is fully fusing in melting pool, and the material road gets into settling pond through rising;
Step 2: liquid glass is clarified in settling pond, eliminates the inner bubble of glass;
Step 3: liquid glass gets into the platinum work pool, adopts platinum agitator liquid towards glass to stir;
Step 4: liquid glass flows out through the platinum discharge nozzle, obtains K9 opticglass.
3. according to the said a kind of K9 opticglass preparation method of claim 2, it is characterized in that: melting pool adopts three-phase alternating current to the raw material direct heating in the said step 1.
4. according to the said a kind of K9 opticglass preparation method of claim 2, it is characterized in that: melting pool top is provided with the raw material layer in the said step 1, when reinforced, feeds in raw material through liquid level appearance monitoring level fluctuation amplitude.
5. according to the said a kind of K9 opticglass preparation method of claim 2, it is characterized in that: raw material and grog add in the 4:1 ratio in the reinforced process of said step 1, add raw material earlier, add grog again.
6. according to the said a kind of K9 opticglass preparation method of claim 2, it is characterized in that: settling pond adds finings in the said step 2, and finings adopts Sb
2O
3
7. according to the said a kind of K9 opticglass preparation method of claim 2, it is characterized in that said raw material are by SiO2, BaCO
3, KCO
3, Na
2CO
3, ZnO, H
3BO
3, CaCO
3, Sb
2O
3Form, said grog is the product of raw material gained after step 1-4 processing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101832406A CN102351419A (en) | 2011-07-01 | 2011-07-01 | K9 optical glass and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101832406A CN102351419A (en) | 2011-07-01 | 2011-07-01 | K9 optical glass and preparation method thereof |
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|---|---|
| CN102351419A true CN102351419A (en) | 2012-02-15 |
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817267A (en) * | 2015-04-24 | 2015-08-05 | 湖北戈碧迦光电科技股份有限公司 | Crystal glass and preparation method thereof |
| CN106430910A (en) * | 2016-10-12 | 2017-02-22 | 湖北新华光信息材料有限公司 | Optical glass furnace and melting method |
| CN112745025A (en) * | 2020-12-31 | 2021-05-04 | 苏州卡利肯新光讯科技有限公司 | Potassium barium glass for lens and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050151116A1 (en) * | 2002-05-16 | 2005-07-14 | Schott Ag | Uv-blocking borosilicate glass, the use of the same, and a fluorescent lamp |
| CN101296872A (en) * | 2005-10-31 | 2008-10-29 | 株式会社小原 | Optical glass, apparatus for producing optical glass, and process for producing the same |
-
2011
- 2011-07-01 CN CN2011101832406A patent/CN102351419A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050151116A1 (en) * | 2002-05-16 | 2005-07-14 | Schott Ag | Uv-blocking borosilicate glass, the use of the same, and a fluorescent lamp |
| CN101296872A (en) * | 2005-10-31 | 2008-10-29 | 株式会社小原 | Optical glass, apparatus for producing optical glass, and process for producing the same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104817267A (en) * | 2015-04-24 | 2015-08-05 | 湖北戈碧迦光电科技股份有限公司 | Crystal glass and preparation method thereof |
| CN106430910A (en) * | 2016-10-12 | 2017-02-22 | 湖北新华光信息材料有限公司 | Optical glass furnace and melting method |
| CN106430910B (en) * | 2016-10-12 | 2019-06-18 | 湖北新华光信息材料有限公司 | A kind of optical glass smelting furnace and melting method |
| CN112745025A (en) * | 2020-12-31 | 2021-05-04 | 苏州卡利肯新光讯科技有限公司 | Potassium barium glass for lens and preparation method and application thereof |
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Application publication date: 20120215 |