CN1820885A - Vacuum seal welding method for window and optic window of low temperature metal Dewar - Google Patents

Vacuum seal welding method for window and optic window of low temperature metal Dewar Download PDF

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Publication number
CN1820885A
CN1820885A CN 200610025044 CN200610025044A CN1820885A CN 1820885 A CN1820885 A CN 1820885A CN 200610025044 CN200610025044 CN 200610025044 CN 200610025044 A CN200610025044 A CN 200610025044A CN 1820885 A CN1820885 A CN 1820885A
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Prior art keywords
window
optical window
welding
groove
kovar alloy
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CN 200610025044
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CN100364707C (en
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王小坤
张亚妮
朱三根
刘向阳
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Shanghai Institute of Technical Physics of CAS
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Shanghai Institute of Technical Physics of CAS
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Abstract

The present invention discloses the method of low temperature vacuum sealing and welding between the window frame and the optical window of metal Dewar. In the welding between the window frame of kovar alloy material and the optical window of infrared transmitting material, the optical window is first vacuum plated to form Cr/Au coating as the transition layer in the parts to be welded, and the welding in performed with In as welding material at low temperature. The present invention has the outstanding advantage of low temperature welding producing no negative effect on the antireflective coating in the infrared window. Using soft In as the welding material can buffer the difference between the optical window material and the kovar alloy material in expansion coefficient. The metal Dewar has gas leakage rate superior to 3E(-12) torr.liter/sec and gas releasing rate far lower than that of traditional technological process.

Description

The vacuum seal welding method of the window-frame of low-temperature metal Dewar and optical window
Technical field
The present invention relates to a kind of low-temperature metal Dewar welding procedure that is used for infrared focal plane detector, specifically be meant the vacuum seal welding method of the window-frame and the optical window of low-temperature metal Dewar.
Background technology
High vacuum low-temperature metal Dewar is the critical component that guarantees low temperature infrared focal plane detector operate as normal.Infrared radiation signal is that the infrared optical window by the low-temperature metal Dewar incides on the infrared focal plane detector, transfers radiation signal to signal of telecommunication output by infrared focal plane detector.Infrared optical window is processed into through optics by materials such as glass, quartz, germanium, silicon, zinc sulphide, zinc selenide, sapphires, it and metal Dewar are by kovar alloy window-frame sealed connection, the quality of its sealing and mechanical strength will directly influence the vacuum of Dewar, and then influence the performance of device.
At present, the vacuum seal of kovar alloy window-frame and infrared optical window connects two kinds of methods usually: a kind of is to adopt low-melting PbO-SiO 2, PbO-B 2O 3-SiO 2, B 2O 3, Li 2O-B 2O 3, Na 2O-P 2O 5, B 2O 3-P 2O 5, P 2O 5-SnO-ZnO is that glass is that scolder directly welds, its advantage is that mechanical strength is good, and shortcoming is because airborne hydrogen and helium are that scolder has infiltration to glass, and permeability increases by exponential relationship with the rising of temperature, therefore, the long-term vacuum leakproofness of Dewar is bad.Another kind is to adopt the splicing of low temperature organic gel, and the advantage of this method is that technology is simple, but owing to the meeting under vacuum of low temperature organic gel continues venting, meeting pollution detection device, the while is non-refractory (≤80 ℃) again, is difficult to the vacuum that keeps Dewar interior for a long time.Therefore, the encapsulating method of existing kovar alloy window-frame and infrared optical window is all undesirable, must explore the long-term vacuum seal connection that a kind of new method realizes kovar alloy window-frame and infrared optical window.
Summary of the invention
Purpose of the present invention is exactly the method that the long-term vacuum seal connection of a kind of kovar alloy window-frame and infrared optical window will be provided.
The present invention adopts welding method to connect, and its step is as follows:
1. adopt conventional photoetching and masking method to use ion beam sputtering method on the ring surface infrared optical window 1 and kovar alloy window-frame 2 grooves contacting mutually, sputter chromium layer 101 successively, thickness is the 300-400 dust; Gold layer 102, thickness is 1 μ m.Vacuum evaporation antireflective coating 203 on the non-solder side of infrared optical window then.
2. press indium ring 3 of shape and size processing of kovar alloy window-frame groove 201, the height of indium ring will be higher than depth of groove 0.02-0.04mm.
3. in kovar alloy window-frame groove, evenly coat the ethylene glycol saturated solution of zinc chloride; as scaling powder; the above-mentioned indium ring that processes is placed in the groove as scolder; put it into again on the electric furnace 4; cover on the electric furnace with cover; charge into nitrogen; under protection of nitrogen gas, be heated to 160-170 ℃, kept 5-6 minute; at this moment; melt solder and very full filling up in the groove stop heating then, reduce to room temperature naturally; it is immersed swing in the absolute ethyl alcohol again and wash, under nitrogen protection, be heated to 35-40 ℃ of oven dry again.
4. the printing opacity position of the optical window that step 1 is prepared is protected with photoresist; antireflective coating on the protection infrared window; on the belt gold layer 102 at optical window edge, evenly be coated with the alcohol saturated solution of last layer rosin; optical window is put on the kovar alloy window-frame groove; the interior indium of the belt gold layer that makes optical window and groove contacts; on optical window, add a ponderable briquetting 5 then; put it into again in the heating furnace 4; charge into nitrogen; under protection of nitrogen gas, be heated to 160-170 ℃, kept 10 minutes; at this moment, melt solder and scolder close with golden laminating fully.After dropping to room temperature, wash, remove photoresist, under nitrogen protection, be heated to 40 ℃ of oven dry again swinging in its immersion absolute ethyl alcohol.The welding of kovar alloy window-frame and infrared optical window finishes.
Advantage of the present invention is as follows:
1. whole welding process is to carry out under lower temperature, is no more than 170 ℃, can not produce any harmful effect to the antireflective coating on the infrared optical window.
2. adopt the soft metal indium to link as scolder, can cushion the difference of the optical window material and the kovar alloy material coefficient of expansion, its leak rate is better than 3 * 10 -12Torr. liter/second; The relative traditional handicraft of venting rate is much smaller.
Description of drawings
Fig. 1 is kovar alloy window-frame of the present invention and infrared optical window welded structure schematic diagram.
Fig. 2 is the partial enlarged drawing of Fig. 1.
Fig. 3 is LONG WAVE INFRARED transmitance situation before and after the welding of germanium optical window.
Fig. 4 is medium wave infrared transmittivity situation before and after the welding of zinc sulphide optical window.
Fig. 5 is a short-wave infrared transmitance situation before and after the quartzy optical window welding.
Fig. 6 is a Visible-to-Near InfaRed transmitance situation before and after the welding of jewel sheet optical window.
The specific embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail:
Infra-red transmitting window gate material at present commonly used has: glass, quartz, germanium, silicon, zinc sulphide, zinc selenide, sapphire.Since not high on these material of infrared window matrixes to the infrared light transmitance, often to form antireflective coating at its two surperficial printing opacities position.At these characteristics, the present invention prevents photoetching and the ion beam sputtering influence to quality of reflection reduction film, at first adopt conventional photoetching and masking method on the groove 201 contacted ring surfaces of infrared optical window 1 and kovar alloy window-frame 2, to use ion beam sputtering method, sputter chromium layer 101 successively, thickness is the 300-400 dust; Gold layer 102, thickness is 1 μ m, as transition zone, its fastness can satisfy welding requirements.Vacuum evaporation antireflective coating 103 on the non-solder side of infrared optical window then.
Adopt the soft metal indium to link as scolder, purpose is the difference that can alleviate the optical window material and the kovar alloy material coefficient of expansion.Secondly welding temperature is low, can not produce any harmful effect to the antireflective on the infrared optical window.
The measurement result of the embodiment of several employing above-mentioned steps welding is provided below:
Embodiment 1: germanium optical window (LONG WAVE INFRARED is added up with the welding of window sample with seasat)
From Fig. 3 as seen, significant change does not take place in transmitance before and after the welding of germanium optical window.Carry out leak rate with leak detector and detect, situation is as follows:
Sample number 1 2 3 4 5 6 7
Leak rate (Torr.l/s) 1.5E-12 1E-12 7E-13 6.42E-13 5.62E-13 7.5E-13 2.0E-12
Embodiment 2: zinc sulphide optical window (No. seven satellite is added up with the welding of medium wave infrared window sample)
From Fig. 4 as seen, significant change does not take place in transmitance before and after the welding of zinc sulphide optical window.Carry out leak rate with leak detector and detect, situation is as follows:
Sample number 1 2 3 4 5 6 7 8
Leak rate (Torr.l/s) 2.4E-12 2.6E-12 1.6E-13 5.6E10-13 1.2E10-12 1.7E10-12 7.5E-13 7.0E-13
Embodiment 3: quartzy optical window (adding up with the welding of short-wave infrared window sample with No. seven satellites)
From Fig. 5 as seen, significant change does not take place in transmitance before and after the quartzy optical window welding.Carry out leak rate with leak detector and detect, situation is as follows:
Sample number 1 2 3 4 5 6 7 8 9
Leak rate (Torr.l/s) 1.9E-12 2.0E-12 6.6E-13 2.0E-12 5.3E-12 3E-12 9.0E-13 7.5E-13 1E-12
Embodiment 4: jewel sheet optical window:
From Fig. 6 as seen, significant change does not take place in transmitance before and after the welding of jewel sheet optical window.Carry out leak rate with leak detector and detect, situation is as follows:
Sample number 1 2 3
Leak rate (Torr.l/s) 6.82E-13 2.2E-12 1.2E-12

Claims (1)

1. the vacuum seal welding method of the window-frame of a low-temperature metal Dewar and optical window is characterized in that concrete steps are as follows:
A. at first adopt conventional photoetching and masking method, on infrared optical window (1) and ring surface that kovar alloy window-frame (2) groove (201) welds mutually, use ion beam sputtering method, sputter chromium layer (101) successively, thickness is the 300-400 dust; Gold layer (102), thickness is 1 μ m; Vacuum evaporation antireflective coating (203) on the non-solder side on infrared optical window surface then;
B. press a shape and size processing indium ring (3) of kovar alloy window-frame groove (201), the height of indium ring will be higher than depth of groove 0.02-0.04mm;
C. in kovar alloy window-frame groove (201), evenly coat the ethylene glycol saturated solution of zinc chloride,, the above-mentioned indium ring (3) that processes is placed in the groove as scolder as scaling powder, put it into again in the stove (4), under protection of nitrogen gas, be heated to 160-170 ℃, kept 5-6 minute, at this moment, melt solder and very full filling up in the groove stop heating then, reduce to room temperature naturally, it is immersed swing in the absolute ethyl alcohol again and wash, under nitrogen protection, be heated to 35-40 ℃ of oven dry again;
D. the printing opacity position of the optical window that steps A is prepared is protected with photoresist; antireflective coating on the protection infrared window; on the belt gold layer (102) at optical window edge, evenly be coated with the alcohol saturated solution of last layer rosin; optical window is put on the kovar alloy window-frame groove (201); the interior indium of the belt gold layer that makes optical window and groove contacts; on optical window, add a ponderable briquetting (5) then; put it into again in the stove (4); under protection of nitrogen gas; be heated to 160-170 ℃, kept 10 minutes, at this moment; melt solder and scolder close with golden laminating fully; after dropping to room temperature, wash, remove photoresist swinging in its immersion absolute ethyl alcohol; be heated to 40 ℃ of oven dry again under nitrogen protection, the welding of kovar alloy window-frame and infrared optical window finishes.
CNB2006100250445A 2006-03-24 2006-03-24 Vacuum seal welding method for window and optic window of low temperature metal Dewar Expired - Fee Related CN100364707C (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101349593B (en) * 2008-09-03 2010-06-02 中国科学院上海技术物理研究所 Infrared detector dewar component high vacuum holding structure and implementing method thereof
CN101866039A (en) * 2010-07-29 2010-10-20 哈尔滨工业大学 High and low temperature resistant medium wave infrared optical window and manufacturing method thereof
CN102117842A (en) * 2009-12-30 2011-07-06 上海欧菲尔光电技术有限公司 Infrared focal plane detector packaging window and manufacturing method thereof
CN103048052A (en) * 2013-01-05 2013-04-17 昆明物理研究所 Miniature metal Dewar inner tube for guidance
CN103759905A (en) * 2014-01-17 2014-04-30 中国科学院上海技术物理研究所 Device for conducting pressurization leakage detection on split type Dewar welding line at low temperature
CN104607745A (en) * 2014-12-15 2015-05-13 贵州黎阳航空动力有限公司 Swirler vacuum brazing method
CN106124134A (en) * 2016-07-27 2016-11-16 中国科学院长春光学精密机械与物理研究所 Optical window assembly device for detecting leak rate and detection method
CN107522413A (en) * 2017-08-22 2017-12-29 惠州市锦恒工业模具设计合伙企业(普通合伙) The optical window structure making process of sapphire eyeglass and kovar alloy air-tight packaging
CN110625284A (en) * 2019-08-14 2019-12-31 中国电子科技集团公司第十一研究所 Infrared detector Dewar welding method
CN114093954A (en) * 2021-10-27 2022-02-25 中国电子科技集团公司第十一研究所 Infrared detector packaging assembly and infrared detector with same
CN115265032A (en) * 2022-09-30 2022-11-01 北京中科富海低温科技有限公司 Low-temperature heat transfer cold shield and vertical test Dewar

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CN2106333U (en) * 1991-11-25 1992-06-03 何曙安 Liquid nitrogen metal dewar bottle of refrigerating 180 units infrared devices
JP3286735B2 (en) * 1991-12-20 2002-05-27 アネルバ株式会社 Vacuum window
US5260575A (en) * 1993-03-10 1993-11-09 Mitsubishi Denki Kabushiki Kaisha Infrared detector
JPH05326988A (en) * 1992-05-19 1993-12-10 Mitsubishi Electric Corp Infrared detector
CN2240143Y (en) * 1995-11-24 1996-11-13 中国科学院上海技术物理研究所 Variable background refrigeration liquid nitrogen metal dewar bottle for infrared detector
CN2327963Y (en) * 1998-01-07 1999-07-07 中国科学院上海技术物理研究所 Dewar flask for containing low temperature preamplifying assembly of infrared detector
CN2511953Y (en) * 2001-12-07 2002-09-18 中国科学院上海技术物理研究所 Air-tight casing for low temperature multi-element infrared detector
CN1267242C (en) * 2003-11-07 2006-08-02 西安交通大学 Anode welding process for metal-glass and metal-ceram

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101349593B (en) * 2008-09-03 2010-06-02 中国科学院上海技术物理研究所 Infrared detector dewar component high vacuum holding structure and implementing method thereof
CN102117842A (en) * 2009-12-30 2011-07-06 上海欧菲尔光电技术有限公司 Infrared focal plane detector packaging window and manufacturing method thereof
CN101866039A (en) * 2010-07-29 2010-10-20 哈尔滨工业大学 High and low temperature resistant medium wave infrared optical window and manufacturing method thereof
CN103048052A (en) * 2013-01-05 2013-04-17 昆明物理研究所 Miniature metal Dewar inner tube for guidance
CN103759905A (en) * 2014-01-17 2014-04-30 中国科学院上海技术物理研究所 Device for conducting pressurization leakage detection on split type Dewar welding line at low temperature
CN103759905B (en) * 2014-01-17 2016-01-13 中国科学院上海技术物理研究所 A kind of at low temperatures to the device of separated type Dewar weld seam pressurization leakage detection
CN104607745A (en) * 2014-12-15 2015-05-13 贵州黎阳航空动力有限公司 Swirler vacuum brazing method
CN104607745B (en) * 2014-12-15 2016-08-24 贵州黎阳航空动力有限公司 A kind of swirler vacuum brazing method
CN106124134A (en) * 2016-07-27 2016-11-16 中国科学院长春光学精密机械与物理研究所 Optical window assembly device for detecting leak rate and detection method
CN106124134B (en) * 2016-07-27 2018-10-16 中国科学院长春光学精密机械与物理研究所 Optical window component device for detecting leak rate and detection method
CN107522413A (en) * 2017-08-22 2017-12-29 惠州市锦恒工业模具设计合伙企业(普通合伙) The optical window structure making process of sapphire eyeglass and kovar alloy air-tight packaging
CN110625284A (en) * 2019-08-14 2019-12-31 中国电子科技集团公司第十一研究所 Infrared detector Dewar welding method
CN114093954A (en) * 2021-10-27 2022-02-25 中国电子科技集团公司第十一研究所 Infrared detector packaging assembly and infrared detector with same
CN114093954B (en) * 2021-10-27 2024-04-19 中国电子科技集团公司第十一研究所 Infrared detector packaging assembly and infrared detector with same
CN115265032A (en) * 2022-09-30 2022-11-01 北京中科富海低温科技有限公司 Low-temperature heat transfer cold shield and vertical test Dewar
CN115265032B (en) * 2022-09-30 2022-12-13 北京中科富海低温科技有限公司 Low-temperature heat transfer cold shield and vertical test Dewar

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