CN102992809B - Preparation method of titanium oxide antireflection film for transparent alumina ceramic - Google Patents
Preparation method of titanium oxide antireflection film for transparent alumina ceramic Download PDFInfo
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- CN102992809B CN102992809B CN201210549567.5A CN201210549567A CN102992809B CN 102992809 B CN102992809 B CN 102992809B CN 201210549567 A CN201210549567 A CN 201210549567A CN 102992809 B CN102992809 B CN 102992809B
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Abstract
The invention relates to a preparation method of a titanium oxide antireflection film for transparent alumina ceramic. The titanium oxide antireflection film is prepared by taking common transparent alumina ceramic, tetrabutyl titanate (Ti(OC4H9)4), acetic acid (CH3COOH), concentrated nitric acid (NHO3), ethanol (CH3CH2OH) and deionized water (H2O) as raw materials and transparent aluminum ceramic as a substrate by adopting a sol-gel method through adjusting the parameters, such as the number of layers of coating films, the annealing temperature and titanium ion concentration. The novel transparent alumina ceramic coated with the titanium oxide antireflection film is higher in light transmittance and favorable in interface bonding, can be used as a core component, namely a light-emitting electric arc tube of a high-voltage sodium lamp, and can be widely applied to the field of illumination, thereby greatly improving the energy source utilization rate, having certain market and favorable industrial prospect and also having greater competitiveness compared with international similar products. Along with in-depth study, the transparent alumina ceramic coated with the titanium oxide antireflection film surely can be applied to the numerous fields and influence social production and life of people.
Description
Technical field
The present invention relates to the preparation method of titanium oxide anti-reflection film for a kind of alumina transparent ceramic, function of dominant ceramic membrane material manufacturing technology field.
Background technology
Transparent alumina is first advanced ceramics material of realizing transparence, in known transparent ceramic material, occupies critical role.Alumina transparent ceramic has the series of advantages such as light transmission, high heat conductance, low conductivity, high rigidity, high strength, low-k and dielectric loss, wear resistance and good corrosion resistance of wide region.These excellent performances make alumina transparent ceramic become gradually the focus of domestic and international research, and obtain increasingly extensive application in fields such as optics, extraordinary instrument manufacturing, electronic technology and high-temperature technology, aerospace and national defense and military industry.Along with high-pressure mercury lamp, halide lamp etc., take geseous discharge and be the development of a main class light source, high temperature and corrosion can not meet the demands the illuminating equipment that originally adopts glass to make fluorescent tube, and high temperature resistant, corrosion resistant aluminum oxide becomes main selection.
From domestic and international research history, since people's invention alumina transparent ceramics such as the R.L. Coble of nineteen fifty-nine GE company, this kind of porcelain tube is widely used on high-pressure mercury lamp always.Use crystalline ceramics pipe as arctube material, tool has the following advantages:
(1) alumina transparent ceramic at high temperature can corrode by resistance to sodium vapor, is the material that high-pressure mercury lamp electric arc tube can not be substituted at present.Because design of material is reasonable, there is not chemical reaction at 1150 ℃ in the alumina transparent ceramic pipe of high-quality and metal halide, thereby can effectively improve the vapour pressure in fluorescent tube below again, makes the light efficiency of lamp and colour rendering index increase.
(2) because the interior luminophore of alumina transparent ceramic and pipe reacts hardly, thereby ceramic gold-halogen lamp is very little in the colour temperature drift of life period, photochromic stable.
(3), due to the stability under alumina-ceramic high temperature, the loss of the interior luminophore of electric arc tube is very slow, thereby the length of comparing with other light sources the work-ing life of high-pressure mercury lamp.
(4) geometric accuracy of ceramic arc tube is high, and deviation is little, and the consistency of performance of lamp is good.
Within 1962, R.L. Coble reported first has successfully been prepared transparent alumina ceramic material, for stupalith has been opened up new Application Areas.Although preparing the technology of the high-strength alumina transparent ceramic of pore-free, existing laboratory is gradually improved, but alumina transparent ceramic light transmission is always not high, further expansion along with its range of application, people will inevitably propose more and more higher performance requriements, and this just requires constantly to go the novel aluminum oxide transparent ceramic material of developing high transmission rate to meet people's demand.
The present invention is with on the basis of common alumina transparent ceramic, be intended to further improve its transmittance, by sol-gel method, prepare titanium oxide anti-reflection film, after adopting special process to process, film and substrate interface bonding force are strong, can significantly improve the transmittance of alumina transparent ceramic.This technological process is simple, and raw material sources are wide and cheap, and product can be widely used in lighting field, improves energy utilization rate, for the production of factory, has very important significance.Alumina transparent ceramic has certain market and good industrialization prospect, its at home and abroad the competitive power in like product also will greatly improve.
Summary of the invention
The object of this invention is to provide the preparation method of titanium oxide anti-reflection film for a kind of alumina transparent ceramic, on common alumina transparent ceramic basis, further improve its transmittance, the operational path of applicable industrialization, modern production is provided.
For achieving the above object, the present invention is by the following technical solutions:
The preparation method of titanium oxide anti-reflection film for alumina transparent ceramic, comprises the steps:
(1) take common alumina transparent ceramic as substrate, adopt tetrabutyl titanate (Ti (OC
4h
9)
4), acetic acid (CH
3cOOH), concentrated nitric acid (HNO
3), ethanol (CH
3cH
2oH), deionized water (H
2o) be raw material;
(2) a certain amount of deionized water is mixed fully with acetic acid, fully stir, make A solution, with nitric acid, regulating A solution to make pH value is 2-5; After tetrabutyl titanate is mixed by a certain percentage with dehydrated alcohol, add stirring magnetic, by magnetic stirrer, be designated as B solution, then rapidly A solution poured in B solution, continue constant temperature and stir 2h, form homogeneous transparent colloidal sol, naturally cool to room temperature, ageing 48-72h;
(3) adopt crystal pulling method to prepare film, lowering speed is 400 μ m/s, and substrate dipping time in colloidal sol is 60s, and pull rate is 200 μ m/s;
(4) the prepared wet film 200 ℃ of dry 10min in resistance furnace of crystal pulling method, take out room temperature and are cooled to normal temperature, the lower thin film of preparation;
(5) repeating step (3) and (4), until obtain the required number of plies;
(6) the dry complete film of certain number of plies is warming up to 600-800 ℃ with 5 ℃/min in resistance furnace, is incubated 1h in air atmosphere, furnace cooling, obtains alumina transparent ceramic titanium oxide anti-reflection film.
It is raw material that the present invention adopts common alumina transparent ceramic, tetrabutyl titanate, acetic acid, concentrated nitric acid, ethanol, deionized water, take alumina transparent ceramic as substrate, by regulating the parameters such as coating layers, annealing temperature, titanium ion concentration, adopt sol-gel method to prepare titanium oxide anti-reflection film.This novel alumina transparent ceramic that is coated with titanium oxide anti-reflection film has higher transmittance, interface, in conjunction with good, is used as sodium lamp arc tube, to further raising high-pressure mercury lamp performance, prolongs life, manufactures high-quality alumina transparent ceramic pipe most important.Along with the development of the whole world " carbon economy " pattern, at national energy-saving, reduce discharging under the macroscopic conditions of development energy-conserving product, the high-pressure mercury lamp at home and abroad development space in market is wide, and market capacity is very large.Film forming apparatus of the present invention and technique are simple, is easy to realize, and less investment, instant effect, can increase alumina transparent ceramic value-added content of product dramatically, in the contrast of the international like product of this invention Yu, has larger competitive power.
Accompanying drawing explanation
Fig. 1 is the transmittance of the thin film of titanium oxide of 2 layers of preparation of 0.07mol/L plated film in embodiment 1.
Fig. 2 is the transmittance of the thin film of titanium oxide of 5 layers of preparation of 0.03mol/L plated film in embodiment 2.
Fig. 3 is the transmittance of the thin film of titanium oxide of 3 layers of preparation of 0.01mol/L plated film in embodiment 3.
Fig. 4 is the transmittance comparison diagram of the film that in embodiment 4 prepared by different titanium ion concentrations.
Embodiment
embodiment 1
A certain amount of deionized water is mixed fully with Glacial acetic acid, fully stir, make A solution, with nitric acid, regulating A solution to make pH value is 2-5; According to titanium ion concentration, be 0.07mol/L, after tetrabutyl titanate is mixed by a certain percentage with dehydrated alcohol, add stirring magnetic, by magnetic stirrer, be designated as B solution, then rapidly A solution is poured in B solution, continue constant temperature and stir 2h, form homogeneous transparent colloidal sol, naturally cool to room temperature, ageing 48-72h.Adopt crystal pulling method to prepare film, lowering speed is 400 μ m/s, and substrate dipping time in colloidal sol is 60s, and pull rate is 200 μ m/s, plating 2 layer films, and annealing temperature is 700 ℃, the time is 1h.
The prepared alumina transparent ceramic of the present embodiment is used titanium oxide anti-reflection film transmittance test result as shown in Figure 1.
A certain amount of deionized water is mixed fully with Glacial acetic acid, fully stir, make A solution, with nitric acid, regulating A solution to make pH value is 2-5; According to titanium ion concentration, be 0.03mol/L, after tetrabutyl titanate is mixed by a certain percentage with dehydrated alcohol, add stirring magnetic, by magnetic stirrer, be designated as B solution, then rapidly A solution is poured in B solution, continue constant temperature and stir 2h, form homogeneous transparent colloidal sol, naturally cool to room temperature, ageing 48-72h.Adopt crystal pulling method to prepare film, lowering speed is 400 μ m/s, and substrate dipping time in colloidal sol is 60s, and pull rate is 200 μ m/s, plating 5 layer films, and annealing temperature is 600 ℃, the time is 1h.
The prepared alumina transparent ceramic of the present embodiment is used titanium oxide anti-reflection film transmittance test result as shown in Figure 2.
A certain amount of deionized water is mixed fully with Glacial acetic acid, fully stir, make A solution, with nitric acid, regulating A solution to make pH value is 2-5; According to titanium ion concentration, be 0.01mol/L, after tetrabutyl titanate is mixed by a certain percentage with dehydrated alcohol, add stirring magnetic, by magnetic stirrer, be designated as B solution, then rapidly A solution is poured in B solution, continue constant temperature and stir 2h, form homogeneous transparent colloidal sol, naturally cool to room temperature, ageing 48-72h.Adopt crystal pulling method to prepare film, lowering speed is 400 μ m/s, and substrate dipping time in colloidal sol is 60s, and pull rate is 200 μ m/s, plating 3 layer films, and annealing temperature is 800 ℃, the time is 1h.
The prepared alumina transparent ceramic of the present embodiment is used titanium oxide anti-reflection film transmittance test result as shown in Figure 3.
embodiment 4
A certain amount of deionized water is mixed fully with Glacial acetic acid, fully stir, make A solution, with nitric acid, regulating A solution to make pH value is 2-5; According to titanium ion concentration, be 0.4mol/L, 0.6mol/L, 0.8mol/L, 1.0mol/L respectively, after tetrabutyl titanate is mixed by a certain percentage with dehydrated alcohol, add stirring magnetic, by magnetic stirrer, be designated as B solution, then rapidly A solution is poured in B solution, continue constant temperature and stir 2h, form homogeneous transparent colloidal sol, naturally cool to room temperature, ageing 48-72h.Adopt crystal pulling method to prepare film, lowering speed is 400 μ m/s, and substrate dipping time in colloidal sol is 60s, and pull rate is 200 μ m/s, plating 2 layer films, and annealing temperature is 700 ℃, the time is 1h.
The prepared alumina transparent ceramic of the present embodiment is used titanium oxide anti-reflection film transmittance test result as shown in Figure 4.
Claims (1)
1. the preparation method of titanium oxide anti-reflection film for alumina transparent ceramic, is characterized in that, comprises the steps:
(1) take common alumina transparent ceramic as substrate, adopting tetrabutyl titanate, acetic acid, concentrated nitric acid, ethanol and deionized water is raw material;
(2) a certain amount of deionized water is mixed fully with acetic acid, fully stir, make A solution, with concentrated nitric acid, regulating A solution to make pH value is 2-5; According to titanium ion concentration 0.01-0.1mol/L, after tetrabutyl titanate is mixed by a certain percentage with ethanol, add stirring magnetic, by magnetic stirrer, be designated as B solution, then rapidly A solution is poured in B solution, continue constant temperature and stir 2h, form homogeneous transparent colloidal sol, naturally cool to room temperature, ageing 48-72h;
(3) adopt crystal pulling method to prepare film, lowering speed is 400 μ m/s, and substrate dipping time in colloidal sol is 60s, and pull rate is 200 μ m/s;
(4) the wet film that prepared by step (3) 200 ℃ of dry 10min in resistance furnace, take out and are at room temperature cooled to normal temperature, the lower thin film of preparation;
(5) repeating step (3) and (4), until obtain the required number of plies;
(6) the dry complete film of certain number of plies is warming up to 600-800 ℃ with 5 ℃/min in resistance furnace, is incubated 1h in air atmosphere, furnace cooling, obtains alumina transparent ceramic titanium oxide anti-reflection film.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105016775A (en) * | 2015-07-03 | 2015-11-04 | 常州明尔瑞陶瓷有限公司 | Method for preparing silicon oxide antireflection coating on alumina transparent ceramic substrate |
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| US9287106B1 (en) | 2014-11-10 | 2016-03-15 | Corning Incorporated | Translucent alumina filaments and tape cast methods for making |
| CN104987136B (en) * | 2015-07-03 | 2017-04-19 | 常州明尔瑞陶瓷有限公司 | Method for preparing titanium oxide/silicon oxide antireflection film on aluminum oxide transparent ceramic substrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105016775A (en) * | 2015-07-03 | 2015-11-04 | 常州明尔瑞陶瓷有限公司 | Method for preparing silicon oxide antireflection coating on alumina transparent ceramic substrate |
| CN105016775B (en) * | 2015-07-03 | 2017-08-25 | 常州明尔瑞陶瓷有限公司 | The method that silica anti-reflection film is prepared in alumina transparent ceramic substrate |
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