CN1013624B - Prodn. method of high-efficiency vacuum ultraviolet source - Google Patents
Prodn. method of high-efficiency vacuum ultraviolet sourceInfo
- Publication number
- CN1013624B CN1013624B CN 89106035 CN89106035A CN1013624B CN 1013624 B CN1013624 B CN 1013624B CN 89106035 CN89106035 CN 89106035 CN 89106035 A CN89106035 A CN 89106035A CN 1013624 B CN1013624 B CN 1013624B
- Authority
- CN
- China
- Prior art keywords
- vacuum ultraviolet
- sealing
- ultraviolet source
- magnesium fluoride
- solder glass
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Landscapes
- Vessels And Coating Films For Discharge Lamps (AREA)
- Glass Compositions (AREA)
Abstract
The present invention relates to a manufacturing method of a high-efficiency vacuum ultraviolet source, and radiation with the wave length of smaller than 200 milli-microns is the vacuum ultraviolet radiation. In the manufacturing method of a high-efficiency vacuum ultraviolet source, magnesium fluoride capable of penetrating the wave length of larger than 115 milli-microns is used as an output window piece, and welding glass slurry is prepared from welding glass powder. An electrode as a polar direct-current discharge vacuum ultraviolet source is sealed with a magnesium fluoride single-crystal piece, or outer shell glass as a non-polar high-frequency discharge vacuum ultraviolet source is sealed with the magnesium fluoride single-crystal piece. The two ultraviolet sources are both filled with mixed gas, and therefore, the manufactured vacuum ultraviolet source can have high light emitting power. The present invention has the advantages of simple sealing method, easily mastered technique, simple appliance and high rate of finished products, and the present invention also enhances the mechanical strength and the physical and chemical property of the manufactured vacuum ultraviolet source.
Description
The present invention relates to a kind of manufacture method of high-efficiency vacuum ultraviolet source.
Vacuum ultraviolet light source can give off wavelength less than 200 millimicrons deep UV (ultraviolet light).Charge into pure hydrogen or pure krypton gas in the conventional vacuum uviol lamp, lamp is promptly at pure hydrogen or pure krypton electric discharge machining in gas.Though so also can obtain the resoance radiation of 10.2ev, but when pure hydrogen or the discharge of pure krypton gas, produce a large amount of ground state hydrogen atoms or ground state krypton atom, resoance radiation is had strong absorption, this absorption is called self-absorption, and it can reduce the vacuum ultraviolet (VUV) output of 10.2ev.Reduce the amount that charges into hydrogen or krypton gas, can reduce self-absorption, but can produce the also corresponding minimizing of excimer subnumber of radiation, can reduce the power output of vacuum ultraviolet light source like this.In addition, because vacuum ultraviolet can not see through common transparent materials such as glass, has only magnesium fluoride (MgF
2) wait the monocrystal of some metal halides could see through vacuum ultraviolet.With the window of magnesium fluoride as vacuum ultraviolet, it and the glass of light shell outer cover or the vacuum tight sealing-in of metal electrode at present, mechanical strength is not high, easily comes off, and vacuum tight does not reach 10
-5-10
-6The requirement of torr, thermal stability and poor chemical stability are unable to undergo the baking of high-temperature slightly, and complex process, and technology is difficult to grasp the cost height.
The objective of the invention is the manufacture method of above-mentioned vacuum ultraviolet light source is improved, providing a kind of has higher ultraviolet output and has the manufacture craft of the vacuum ultraviolet light source of good sealing property.
The present invention includes and adopt the window of magnesium fluoride single-chip as the output window of vacuum ultraviolet light source, charge into the steps such as mist of proper proportion with the method for sealing between magnesium fluoride single-chip and glass lamp housing or the metal electrode, in the good vacuum UV lamp of sealing-in with seal, sealing materials, obtain having the 10.2ev vacuum ultraviolet light source of higher ultraviolet output.The vacuum ultraviolet wavelength is less than 200 millimicrons, and magnesium fluoride can see through wavelength greater than 115 millimicrons vacuum ultraviolet, and has excellent mechanical intensity, and stable physical and chemical performance is good vacuum ultraviolet light source output window sheet material.Solder glass component as seal, sealing materials is as follows:
Lead oxide (PbO): 1 magnesium oxide (MgO): 0.05-0.15
Diboron trioxide (B
2O
3): 0.14-0.2 silicon dioxide (SiO
2): 0.05-0.1
Zinc oxide (ZnO): 0.1-0.15 yttria (Y
2O
3): 0.01-0.05
Crystallization was the crystallite attitude after zinc oxide can impel solder glass seal in the component, improve the closure resistance to elevated temperatures, magnesium oxide can be adjusted the coefficient of linear expansion of solder glass, adds an amount of yttria, can improve the wettability of solder glass and closure, guarantee the vacuum tight degree.The solder glass coefficient of linear expansion of this composition is close with the magnesium fluoride single-chip.During sealing-in, above-mentioned solder glass powder and guncotton solution are mixed with solder glass powder slurry, in 420-480 ℃ of temperature range, carry out sealing-in.Charge into before the mist, earlier air in the lamp is evacuated to 10
-5-10
-6Torr, baking fluorescent tube 1 hour under 400 ℃ of temperature, be cooled to charge in the following mist after the room temperature any:
(a) 1-10% hydrogen adds 90-99% helium or neon to the 0.5-10 torr,
(b) 1-10% krypton gas adding 90-99% helium or neon are to the 0.5-10 torr.
Among the present invention, if will obtain the sealing property of requirements at the higher level, above-mentioned solder glass can adopt following component:
Lead oxide (PbO): 1 magnesium oxide (MgO): 0.08-0.12
Diboron trioxide (B
2O
3): 0.15-0.19 silicon dioxide (SiO
2): 0.06-0.09
Zinc oxide (ZnO): 0.12-0.15 yttria (Y
2O
3): 0.01-0.03
Among the present invention, more suitable sealing temperature scope is 440 ± 15 ℃.
Method for sealing of the present invention can be used for the vacuum ultraviolet light source of two kinds of structures, and a kind of is the direct-current discharge type, and it has two electrodes, and magnesium fluoride monocrystalline window is enclosed on the metal electrode; Second kind is electrodeless high-frequency discharge, and magnesium fluoride monocrystalline window is enclosed on the glass shell.Must be close by the coefficient of linear expansion of closure with the coefficient of linear expansion of magnesium fluoride monocrystal, generally adopt the glass shell of platinum group glass as electrodeless high-frequency discharge light source.Adopt stainless steel as the electrode that electrode direct-current discharge light source is arranged, can make closure that good vacuum-tightness, chemical stability, high temperature resistant and be convenient to processing are arranged like this.
Embodiment:
Because the magnesium fluoride monocrystal is anisotropic, its coefficient of linear expansion α is respectively 13.1 * 10 on vertical C axle and parallel C axle both direction
-6/ ℃ and 8.8 *
-6/ ℃, differ a lot of.In order to make magnesium fluoride and close coefficient of linear expansion to be arranged by the glass of sealing-in or metal electrode, need the directed cutting of magnesium fluoride crystal, the magnesium fluoride monocrystalline of using as window is downcut by vertical C direction of principal axis, obtain having on the plane magnesium fluoride wafer of even, constant coefficient of linear expansion like this, can carry out the matched seal of flat envelope form.The window that cuts down will be through polishing, and it is stand-by to be polished to 1/2 aperture.DB403 glass is made the light source shell material in the employing platinum group glass, and its coefficient of linear expansion is 8.9 * 10
-6/ ℃.As electrode material, its coefficient of linear expansion is 10 * 10 with stainless steel 12 chromium
-6/ ℃.When magnesium fluoride and glass are done sealing-in, glass tube be cut short, polish, use the residue of ultrasonic wave flush away frosted again, oven dry.When magnesium fluoride and metal electrode were done sealing-in, sealing surface needed smooth, and will remove the greasy dirt of metal sealing face with acetone, cleaned with distilled water then.During sealing-in, earlier solder glass powder 10 grams are added guncotton solution (100 milliliters of butyl acetates add 7 gram nitrocottons) 4-6 milliliter and be made into sealing-in place for the treatment of that solder glass powder slurry is applied to two closures respectively, Deng glass dust slurry dried slightly after, add again and be coated with some powder slurries, then two closures are closed up, pressurization 100 grams place Muffle furnace to rise to 440 ℃ with about 100 ℃/hour programming rate, insulation is handled then, is cooled to room temperature with 100 ℃/hour speed and gets final product.
Have utmost point direct-current discharge lamp or electrodeless high-frequency lamp that sealing-in finishes connect vacuum-pumping system, are evacuated to 10
-5-10
-6Torr, baking is 1 hour under 400 ℃ of temperature, takes out and is cooled to room temperature, charges into 2% hydrogen and 98% neon to 0.5 torr in utmost point direct-current discharge lamp is arranged.In electrodeless high-frequency discharge lamp, charge into 2% krypton gas and 98% helium to 1 torr.
By above manufacture craft, can obtain high efficiency have utmost point direct-current discharge and two kinds of vacuum ultraviolet light sources of electrodeless high-frequency discharge.
The electrodeless vacuum UV lamp structure chart of accompanying drawing 1 for making with the inventive method, the structure chart that utmost point direct-current discharge vacuum UV lamp arranged of accompanying drawing 2 for making with the inventive method, wherein 1 is the magnesium fluoride single-chip, the 2nd, solder glass, the 3rd, the glass shell of electrodeless lamp, the 4th, stainless steel electrode, the 5th, can cut down.
Vacuum ultraviolet light source with this method makes owing to reduced the amount of ground state hydrogen atom or krypton atom, has reduced self-absorption, has improved the power output of vacuum ultraviolet light source, and the photon output of this vacuum ultraviolet light source can reach 1011Photons/second. Use sealing technology of the present invention, because the solder glass linear expansion coefficient is close with closure, and the temperature variant curve of linear expansion coefficient is also close with closure, therefore can guarantee matched seal, during solder glass seal, surface tension is very little, therefore with closure good wellability is arranged, and makes sealing-in place that good vacuum tight be arranged. Solder glass crystallization after the sealing-in is the crystallite attitude, and softening temperature is brought up to more than 500 ℃, and fluorescent tube can be toasted under 400 ℃ of temperature repeatedly. This method for sealing is easy, and temperature control Muffle furnace of device just, sealing technology are easy to grasp, and during sealing-in the control of temperature, the viscosity of glass powder paste is required all can obtain satisfied result in wider control range. Vacuum ultraviolet light source mechanical strength and the physical and chemical stability made with the inventive method all improve a lot.
Direct-current discharge type and the electrodeless high-frequency discharge type vacuum ultraviolet light source made with the inventive method can be widely used in the technology such as photo-ionisation, optical excitation, light decomposition, light compositing.
Claims (3)
1, a kind of manufacture method of high-efficiency vacuum ultraviolet source comprises and adopts the window of magnesium fluoride monocrystalline as the ultraviolet source output window, will charge into mist etc. in window and glass housing or metal electrode sealing-in and the lamp with seal, sealing materials, it is characterized in that:
(1) above-mentioned seal, sealing materials adopts the solder glass of being made up of following component:
Lead oxide (PbO): 1 magnesium oxide (MgO): 0.05-0.15
Diboron trioxide (B
2O
3): 0.14-0.2 silicon dioxide (SiO
2): 0.05-0.1
Zinc oxide (ZnO): 0.1-0.15 yttria (Y
2O
2): 0.01-0.05
(2) during sealing-in, above-mentioned solder glass powder and guncotton solution are mixed with solder glass powder slurry, in 420-480 ℃ of temperature range, carry out sealing-in;
(3) above-mentioned mist is following any:
(a) 1-10% hydrogen adds 90-99% helium or neon to the 0.5-10 torr,
(b) 1-10% krypton gas adding 90-99% helium or neon are to the 0.5-10 torr.
2, the manufacture method of vacuum ultraviolet light source according to claim 1 is characterized in that the solder glass that seal, sealing materials adopts following component to form:
Lead oxide (PbO): 1 magnesium oxide (MgO): 0.08-0.12
Diboron trioxide (B
2O
3): 0.15-0.19 silicon dioxide (SiO
2): 0.06-0.09
Zinc oxide (ZnO): 0.12-0.15 yttria (Y
2O
3): 0.01-0.03
3, the manufacture method of vacuum ultraviolet light source according to claim 1 is characterized in that the sealing temperature scope is 440 ± 15 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89106035 CN1013624B (en) | 1989-11-11 | 1989-11-11 | Prodn. method of high-efficiency vacuum ultraviolet source |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89106035 CN1013624B (en) | 1989-11-11 | 1989-11-11 | Prodn. method of high-efficiency vacuum ultraviolet source |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1043037A CN1043037A (en) | 1990-06-13 |
| CN1013624B true CN1013624B (en) | 1991-08-21 |
Family
ID=4856599
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89106035 Expired CN1013624B (en) | 1989-11-11 | 1989-11-11 | Prodn. method of high-efficiency vacuum ultraviolet source |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1013624B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100413011C (en) * | 2004-08-06 | 2008-08-20 | 于首成 | Health-care UV-lamp |
| CN100533643C (en) * | 2004-12-31 | 2009-08-26 | 中国科学院西安光学精密机械研究所 | Near ultraviolet light input window and manufacturing method thereof |
| CN1319886C (en) * | 2005-01-12 | 2007-06-06 | 吴为新 | Gemstone ceramic sintering agent and method for manufacturing gemstone ceramic products |
| CN103094057B (en) * | 2013-02-01 | 2015-07-22 | 余建军 | Double-wavelength ultraviolet lamp |
| CN106373860B (en) * | 2016-11-18 | 2018-02-27 | 常州玉宇电光器件有限公司 | Middle pressure discharge lamp and its manufacturing process and water process method for disinfection |
| CN114252502A (en) * | 2020-09-22 | 2022-03-29 | 中国科学院大学 | Method for detecting acetonitrile and derivatives thereof in real time by excited methylene chloride induced proton transfer reaction mass spectrum |
-
1989
- 1989-11-11 CN CN 89106035 patent/CN1013624B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN1043037A (en) | 1990-06-13 |
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| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C13 | Decision | ||
| GR02 | Examined patent application | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |