CN104591539A - Borosilicate glass with high transmittance at far ultraviolet band and preparation method thereof - Google Patents
Borosilicate glass with high transmittance at far ultraviolet band and preparation method thereof Download PDFInfo
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- CN104591539A CN104591539A CN201510046650.4A CN201510046650A CN104591539A CN 104591539 A CN104591539 A CN 104591539A CN 201510046650 A CN201510046650 A CN 201510046650A CN 104591539 A CN104591539 A CN 104591539A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
-
- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/0085—Compositions for glass with special properties for UV-transmitting glass
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention relates to the field of glass manufacturing and particularly relates to borosilicate glass with high transmittance at a far ultraviolet band and a preparation method thereof. The borosilicate glass is composed of the following components in percentage by mass: 65-70% of silica, 20-25% of boron oxide, 1-5% of sodium oxide, 0.5-5% of alumina, 0.2-2% of potassium oxide and 0.2-2% of lithium oxide. The preparation method comprises the following steps: weighing materials: weighing the raw material components according to a set proportion and mixing to form a mixture; calcining: calcining the mixture; smelting: smelting the calcined mixture into molten glass under a high temperature condition; molding: carrying out casting molding on the molten glass to obtain a glass block, and annealing the glass block. The borosilicate glass has good chemical stability, small thermal expansion coefficient band, good matching property with a kovar alloy and high transmittance at the far ultraviolet band, the preparation method is simple, and the production cost is low.
Description
Technical field
The present invention relates to glass manufacturing area, especially a kind of borosilicate glass and preparation method thereof.
Background technology
Ultraviolet is from the shorter purple end (wavelength is about 400nm) of visible wavelength, to the electromagnetic radiation spectrum of X-ray (wavelength 10nm).Major part colouless optical glass all has higher transmitance at visible light wave range, but all there is absorption in various degree to ultraviolet band.This is because under high-octane uviolizing, the electronics of colouless optical glass inside is excited, and about 3eV energy level, transition occurs, thus absorbs ultraviolet.
Therefore the glass only having minority to have special composition has good UV-permeable performance, as silica glass, B
2o
3glass and P
2o
5the UV-permeable cutoff wavelength of glass is 160nm, 170nm and 145nm respectively, all has higher ultraviolet permeability.But, due to B
2o
3glass and P
2o
5the performance of each side such as the chemical stability of glass and intensity is difficult to meet application demand, silica glass is only had to have actual application value, but silica glass preparation condition is harsh, softening temperature is high, with the thermal expansivity of the alloy such as valve can differ comparatively large, these problems greatly limit the application of silica glass.
Except silica glass except, polycomponent silicate and polycomponent phosphate glass also can be used as ultraviolet optical material, have some examples of many successful abroad.As Xiao Te 8337b glass and healthy and free from worry 9741 glass, in these glass, introduce a certain amount of Al
2o
3, B
2o
3, R
2o (R is alkalimetal ion), thus make ultraviolet cut-on wavelength (λ 0) higher than 200nm, but glass the average transmittances of whole ultraviolet band or the coefficient of expansion with can the sealing-in of valve alloy not mate.In addition contain fluorochemical and muriate in these glass, in the high temperature melting process of glass, these halogenide cause erosion action to a certain degree to platinum crucible, increase cost and production safety hidden danger.P
2o
5-SiO
2-B
2o
3-GeO
2the glass of system also has UV-permeable performance, but this system glass is containing P
2o
5etc. unstable constituents, the water resistant chemical stability of glass is poor, low strength.
In brief, the deficiency of existing ultraviolet optical glass shows as:
1) transmitance of extreme ultraviolet region is lower.9741 glass specimens as thick in 1.0mm, the transmittance at 190nm place only about 12%, the transmittance at 254nm place only about 70%, 300 ~ 1100nm wave band average transmittances is only 85%.
2) coefficient of expansion fluctuation is large, with can the metal such as valve alloy carry out high intermediate temperature sealing time the coefficient of expansion do not mate, be difficult to meet hermetic seal requirement.Room temperature to a 300 DEG C corresponding coefficient of expansion as 8337b glass is 56 ~ 61 × 10-7/ DEG C, P
2o
5-SiO
2-B
2o
3-GeO
2room temperature to a 300 DEG C corresponding coefficient of expansion for system glass is 58 ~ 77 × 10-7/ DEG C, and can the thermal expansivity of the metal such as valve alloy be 46 ~ 52 × 10-7/ DEG C.
3) glass composition halide or P
2o
5, unfriendly to environment, water resistant chemical stability is poor.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art and a kind of borosilicate glass and preparation method thereof is provided, described borosilicate glass chemical stability is good, thermal expansivity wave band is little and with can valve alloy mates well, extreme ultraviolet region has comparatively high permeability, described preparation method is simple, and production cost is lower.
The object of the invention to solve the technical problems realizes by the following technical solutions.
By a kind of borosilicate glass of extreme ultraviolet region high permeability, composed of the following components by mass percentage:
The borosilicate glass of above-mentioned extreme ultraviolet region high permeability, is made up of following oxide component by mass percentage:
The object of the invention to solve the technical problems can also realize by the following technical solutions.
By a kind of preparation method of above-mentioned borosilicate glass, comprise the following steps:
Weighing step: the raw material of each component is carried out weighing and mixing according to setting proportioning, forms compound;
Calcining step: described compound is carried out calcination processing;
Fusing step: the compound after calcination processing is formed glass metal under the high temperature conditions;
Forming step: be glass block by described glass metal cast molding, by described glass block anneal.
Above-mentioned preparation method, in described calcining step, the condition of described calcination processing is calcination processing 4 ~ 8 hours under 800 ~ 900 DEG C of conditions.
Above-mentioned preparation method, in described fusing step, described hot conditions is melt 4 ~ 8 hours under 1500 ~ 1550 DEG C of conditions.
Above-mentioned preparation method, in described forming step, described anneal condition is under 600 ~ 650 DEG C of conditions, anneals 4 hours, then the described glass block after annealing is down to room temperature with the speed of 0.2 DEG C/min.
Above-mentioned preparation method, in described fusing step, stirs described glass metal, and mixing speed is 10 ~ 50r/min.
Above-mentioned preparation method, in described fusing step, after stirring, clarifies glass metal 6 ~ 10 hours under 1400 ~ 1450 DEG C of conditions.
Above-mentioned preparation method, in described fusing step, continues to pass into high pure nitrogen.
Above-mentioned preparation method, the raw material of described silicon-dioxide is the quartz sand preparation of soaking through hydrochloric acid soln; The raw material of described boron oxide is analytically pure H
3bO
3; The raw material of aluminum oxide is analytically pure Al
2o
3; The raw material of sodium oxide is analytically pure Na
2cO
3; The raw material of potassium oxide is analytically pure K
2cO
3; The raw material of Lithium Oxide 98min is analytically pure Li
2cO
3; Wherein: the iron level of the raw material of each component is all less than 5ppm.
By technique scheme, borosilicate glass of a kind of extreme ultraviolet region high permeability that the present invention proposes and preparation method thereof at least has following advantages:
(1) borosilicate glass adopting this invention to prepare has comparatively high permeability at extreme ultraviolet region, the sample of 1.0mm is as follows in the mistake rate of 190 ~ 1100nm wave band: T%190nm >=46%, T%254nm >=87%, T%300 ~ 1100nm >=90%, significantly improve the transmitance of existing uviol, expand range of application.
(2) the borosilicate glass thermal expansivity prepared of this invention is especially applicable to and can carries out high intermediate temperature sealing by the metal such as valve alloy, the coefficient of expansion of room temperature to 300 DEG C is 48 ~ 52 × 10-7/ DEG C, in addition, this glass has the performance of excellent water resistant chemical stability, bending strength and heat shock resistance.
(3) preparation method of the present invention is simple, and environmentally friendly, do not introduce heavy metal ion or toxic glass fining agent, production cost is lower.Prepared saturating UV-light glass material excellent property, is especially applicable to making ultraviolet spectrometer, geological prospecting, nondestructive test and requires that opticinstrument that ultraviolet-visible light transmission rate is all very high, camera lens are first-class.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technique means of the present invention, and can be implemented according to the content of specification sheets, be described in detail as follows below with preferred embodiment of the present invention.
Embodiment
For understanding the present invention better, illustrate content of the present invention further below in conjunction with embodiment and comparative example, but content of the present invention is not only confined to the following examples.
Embodiment 1
Weighing step: each feed composition is set proportioning according to table 1 and carries out weighing and mixing, forms compound; Wherein, the raw material of described silicon-dioxide is the quartz sand preparation of soaking through hydrochloric acid soln; , particularly, quartz sand is soaked in hydrochloric acid soln 4 hours, obtain quartz sand iron level be less than 5ppm, then clean with deionized water, then proceed to 120 DEG C of oven for drying 8 hours, be the silicon-dioxide that component in the present embodiment adopts.
The raw material of described boron oxide is analytically pure H
3bO
3; The raw material of aluminum oxide is analytically pure Al
2o
3; The raw material of sodium oxide is analytically pure Na
2cO
3; The raw material of potassium oxide is analytically pure K
2cO
3; The raw material of Lithium Oxide 98min is analytically pure Li
2cO
3.
During concrete enforcement, according in table 1, the mass percentage of boron oxide, sodium oxide, aluminum oxide, potassium oxide and Lithium Oxide 98min, is converted into corresponding mol ratio, according to corresponding mol ratio, is scaled corresponding H
3bO
3, sodium carbonate, salt of wormwood and Quilonum Retard quality.Wherein, carbonate is at high temperature all decomposed into oxide compound and carbonic acid gas.Boron oxide is introduced by boric acid, directly takes analytically pure boric acid according to respective quality, and boric acid is at high temperature decomposed into boron trioxide and water vapour.
Calcining step: compound is carried out calcination processing 4 ~ 8 hours at 850 DEG C of retort furnaces.
Fusing step: the compound after calcination processing is formed glass metal under the high temperature conditions; Compound after calcination processing is added in 1550 DEG C of platinum crucibles to melt and form glass metal in 4 hours, in melting process, adopt platinum stirrer to carry out stirrings eliminating bubble to glass metal, mixing speed 50r/min, after stirring by glass metal in 1450 DEG C of clarifying treatment 6 hours.In this melting process, continue to pass into high pure nitrogen in high-temperature melting furnace, described nitrogen makes glass metal and air insulated, prevents the various component of glass metal and air from carrying out chemical reaction, thus reaches the object protected glass metal.
Forming step: by the glass metal cast molding after clarifying treatment, forms glass block, described glass block is put into 600 ~ 650 DEG C of retort furnace anneal 4 ~ 8 hours, be down to room temperature by 0.2 DEG C/min.Namely described borosilicate glass is obtained.
Then, test the coefficient of expansion (× 10-7/ DEG C) of 300 DEG C of described borosilicate glass, water resistant chemical stability, the transmitance (T%) at 190nm place, the transmitance (T%) at 254nm place and 300 ~ 1100nm wave band average transmittances (T%), list test result in Table 1.
In the present embodiment, during mensuration to sample transmitance, all measure with the sample of 1 mm thick.
Wherein, described water resistant chemical stability experiment measures for adopting GB 9622.11-1988 electronic glass water resistant chemical stability testing method.
The iron level of the raw material of each component is all less than 5ppm.Due to, iron level can make the ultraviolet permeability of glass significantly reduce.Thus less iron level can increase the ultraviolet permeability of the borosilicate glass in the present invention.
As the embodiment that can convert, described silicon-dioxide can also be the high-purity silicon dioxide directly bought.
As the embodiment that can convert, described silica material can also be analytically pure silicon-dioxide.
Embodiment 2
By the method repeating embodiment 1 with each component concentration of specifying in following table 1.List test result in Table 1.
Embodiment 3
By the method repeating embodiment 1 with each component concentration of specifying in following table 1.List test result in Table 1.
Embodiment 4
By the method repeating embodiment 1 with each component concentration of specifying in following table 1, but in described fusing step, described hot conditions is melt 8 hours under 1500 DEG C of conditions, and mixing speed is 30r/min, after stirring, is clarified 10 hours by glass metal under 1400 DEG C of conditions.List test result in Table 1.
Embodiment 5
By the method repeating embodiment 4 with each component concentration of specifying in following table 1.List test result in Table 1.
Comparative example 1 and 2
The glass formula composition of comparative example 1 and 2 does not fall into protection scope of the present invention, and preparation technology is identical with embodiment 1, and glass component, melting technology parameter and glass properties are in table 1.As seen from table, there is more bubble in the glass of comparative example 1 and 2, ultraviolet band transmitance is lower, the coefficient of expansion of glass with can the coefficient of expansion of valve alloy depart from comparatively large, cannot application requiring be met.
In comparative example 2, water resistant chemical stability is II level.In glass ingredient due to comparing embodiment 2, glass-former SiO2 content is too low, and meanwhile, network outer body alkali metal content is too high, so glass water resistant chemical stability prepared by the method is II level.
Table 1 glass component, melting technology parameter and glass properties
The borosilicate glass thermal expansivity prepared by the present invention is especially applicable to and can carries out sealing-in (coefficient of expansion of room temperature to 300 DEG C is 48.5 ~ 50.0 × 10 by the metal such as valve alloy
-7/ DEG C), have higher transmitance at 200 ~ 1100nm wave band, excellent water resistant chemical stability, bending strength and thermal shock resistance, over-all properties is all better than existing holvi glass material.Preparation method of the present invention is simple, and do not introduce heavy metal ion and toxic glass fining agent, environmentally friendly, production cost is lower.The borosilicate glass adopting this invention to prepare is excellent in UV-light wave band transmitance, has wide market application foreground in optical systems such as ultraviolet spectrometer, ultraviolet optics camera lenses.
The above, it is only preferred embodiment of the present invention, not do any pro forma restriction to the present invention, any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (10)
1. a borosilicate glass for extreme ultraviolet region high permeability, composed of the following components by mass percentage:
2. the borosilicate glass of extreme ultraviolet region high permeability as claimed in claim 1, is made up of following oxide component by mass percentage:
3. a preparation method for borosilicate glass described in claim 1 or 2, comprises the following steps:
Weighing step: the raw material of each component is carried out weighing and mixing according to setting proportioning, forms compound;
Calcining step: described compound is carried out calcination processing;
Fusing step: the compound after calcination processing is formed glass metal under the high temperature conditions;
Forming step: be glass block by described glass metal cast molding, by described glass block anneal.
4. preparation method as claimed in claim 3, is characterized in that,
In described calcining step, the condition of described calcination processing is calcination processing 4 ~ 8 hours under 800 ~ 900 DEG C of conditions.
5. preparation method as claimed in claim 3, is characterized in that,
In described fusing step, described hot conditions is melt 4 ~ 8 hours under 1500 ~ 1550 DEG C of conditions.
6. preparation method as claimed in claim 3, is characterized in that,
In described forming step, described anneal condition is under 600 ~ 650 DEG C of conditions, anneals 4 hours, then the described glass block after annealing is down to room temperature with the speed of 0.2 DEG C/min.
7. preparation method as claimed in claim 3, is characterized in that,
In described fusing step, stir described glass metal, mixing speed is 10 ~ 50r/min.
8. preparation method as claimed in claim 7, is characterized in that,
In described fusing step, after stirring, glass metal is clarified 6 ~ 10 hours under 1400 ~ 1450 DEG C of conditions.
9. preparation method as claimed in claim 3, is characterized in that,
In described fusing step, continue to pass into high pure nitrogen.
10. preparation method as claimed in claim 3, is characterized in that,
The raw material of described silicon-dioxide is the quartz sand preparation of soaking through hydrochloric acid soln; The raw material of described boron oxide is analytically pure H
3bO
3; The raw material of aluminum oxide is analytically pure Al
2o
3; The raw material of sodium oxide is analytically pure Na
2cO
3; The raw material of potassium oxide is analytically pure K
2cO
3; The raw material of Lithium Oxide 98min is analytically pure Li
2cO
3;
Wherein: the iron level of the raw material of each component is all less than 5ppm.
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111104A (en) * | 2017-06-26 | 2019-01-01 | 中国南玻集团股份有限公司 | Boroalumino silicate glasses and preparation method thereof |
| CN109422459A (en) * | 2017-08-28 | 2019-03-05 | 杭州富阳环宇玻璃厂 | It is a kind of for passing the ultraviolet high transmittance light of optical wand |
| CN109437560A (en) * | 2018-12-28 | 2019-03-08 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of ultraviolet high borosilicate glass and preparation method thereof thoroughly |
| CN111533465A (en) * | 2020-05-18 | 2020-08-14 | 中国建筑材料科学研究总院有限公司 | Anti-halation step glass and preparation method and application thereof |
| DE202020107534U1 (en) | 2020-12-03 | 2021-07-14 | Schott Ag | Borosilicate glass articles |
| CN116573857A (en) * | 2023-07-12 | 2023-08-11 | 山东龙光天旭太阳能有限公司 | Borosilicate glass with high ultraviolet transmittance and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111104A (en) * | 2017-06-26 | 2019-01-01 | 中国南玻集团股份有限公司 | Boroalumino silicate glasses and preparation method thereof |
| CN109111104B (en) * | 2017-06-26 | 2021-11-05 | 中国南玻集团股份有限公司 | Boron-aluminum silicate glass and preparation method thereof |
| CN109422459A (en) * | 2017-08-28 | 2019-03-05 | 杭州富阳环宇玻璃厂 | It is a kind of for passing the ultraviolet high transmittance light of optical wand |
| CN109437560A (en) * | 2018-12-28 | 2019-03-08 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of ultraviolet high borosilicate glass and preparation method thereof thoroughly |
| CN111533465A (en) * | 2020-05-18 | 2020-08-14 | 中国建筑材料科学研究总院有限公司 | Anti-halation step glass and preparation method and application thereof |
| CN111533465B (en) * | 2020-05-18 | 2021-10-26 | 中国建筑材料科学研究总院有限公司 | Anti-halation step glass and preparation method and application thereof |
| DE202020107534U1 (en) | 2020-12-03 | 2021-07-14 | Schott Ag | Borosilicate glass articles |
| EP3950619A2 (en) | 2020-12-03 | 2022-02-09 | Schott AG | Borosilicate glass item |
| CN116573857A (en) * | 2023-07-12 | 2023-08-11 | 山东龙光天旭太阳能有限公司 | Borosilicate glass with high ultraviolet transmittance and preparation method thereof |
| CN116573857B (en) * | 2023-07-12 | 2023-10-27 | 山东龙光天旭太阳能有限公司 | Borosilicate glass with high ultraviolet transmittance and preparation method thereof |
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Application publication date: 20150506 |