CN104900744B - Intermediate-infrared detector and preparation method thereof - Google Patents
Intermediate-infrared detector and preparation method thereof Download PDFInfo
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- CN104900744B CN104900744B CN201510199477.1A CN201510199477A CN104900744B CN 104900744 B CN104900744 B CN 104900744B CN 201510199477 A CN201510199477 A CN 201510199477A CN 104900744 B CN104900744 B CN 104900744B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000758 substrate Substances 0.000 claims abstract description 197
- 150000003839 salts Chemical class 0.000 claims abstract description 89
- 238000002161 passivation Methods 0.000 claims abstract description 26
- 229920002472 Starch Polymers 0.000 claims abstract description 25
- 235000019698 starch Nutrition 0.000 claims abstract description 25
- 239000008107 starch Substances 0.000 claims abstract description 25
- LUMVCLJFHCTMCV-UHFFFAOYSA-M potassium;hydroxide;hydrate Chemical compound O.[OH-].[K+] LUMVCLJFHCTMCV-UHFFFAOYSA-M 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 153
- 238000000137 annealing Methods 0.000 claims description 82
- 239000010409 thin film Substances 0.000 claims description 82
- 238000000151 deposition Methods 0.000 claims description 79
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 77
- 230000008021 deposition Effects 0.000 claims description 77
- 239000010408 film Substances 0.000 claims description 76
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 71
- 238000000034 method Methods 0.000 claims description 52
- 229910052757 nitrogen Inorganic materials 0.000 claims description 46
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 27
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 27
- 239000007864 aqueous solution Substances 0.000 claims description 23
- 238000004140 cleaning Methods 0.000 claims description 23
- 235000012239 silicon dioxide Nutrition 0.000 claims description 22
- 238000012536 packaging technology Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 239000011521 glass Substances 0.000 claims description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 14
- PNZVFASWDSMJER-UHFFFAOYSA-N acetic acid;lead Chemical compound [Pb].CC(O)=O PNZVFASWDSMJER-UHFFFAOYSA-N 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 14
- 239000010703 silicon Substances 0.000 claims description 14
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 13
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 239000005083 Zinc sulfide Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 11
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 11
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 10
- 238000002207 thermal evaporation Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000005566 electron beam evaporation Methods 0.000 claims description 6
- 238000005538 encapsulation Methods 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000010301 surface-oxidation reaction Methods 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 229940046892 lead acetate Drugs 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 30
- 229910052737 gold Inorganic materials 0.000 description 30
- 239000010931 gold Substances 0.000 description 30
- 239000012153 distilled water Substances 0.000 description 26
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 21
- 206010070834 Sensitisation Diseases 0.000 description 21
- 238000007789 sealing Methods 0.000 description 21
- 230000008313 sensitization Effects 0.000 description 21
- 239000002245 particle Substances 0.000 description 16
- 238000012546 transfer Methods 0.000 description 16
- 230000008020 evaporation Effects 0.000 description 15
- 238000001704 evaporation Methods 0.000 description 15
- 238000010438 heat treatment Methods 0.000 description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 238000000224 chemical solution deposition Methods 0.000 description 10
- 238000007747 plating Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000013049 sediment Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- GGYFMLJDMAMTAB-UHFFFAOYSA-N selanylidenelead Chemical compound [Pb]=[Se] GGYFMLJDMAMTAB-UHFFFAOYSA-N 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 238000005057 refrigeration Methods 0.000 description 3
- 239000000052 vinegar Substances 0.000 description 3
- 235000021419 vinegar Nutrition 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005234 chemical deposition Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- IYKVLICPFCEZOF-UHFFFAOYSA-N selenourea Chemical compound NC(N)=[Se] IYKVLICPFCEZOF-UHFFFAOYSA-N 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- PMUIBVMKQVKHBE-UHFFFAOYSA-N [S].NC(N)=O Chemical compound [S].NC(N)=O PMUIBVMKQVKHBE-UHFFFAOYSA-N 0.000 description 1
- XSKUQABTDMBZCN-UHFFFAOYSA-N [Sb].[As].[In] Chemical compound [Sb].[As].[In] XSKUQABTDMBZCN-UHFFFAOYSA-N 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 lead acetate Chemical compound 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229940110728 nitrogen / oxygen Drugs 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000289 photo-effect Toxicity 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 125000003748 selenium group Chemical group *[Se]* 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/08—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
- H01L31/09—Devices sensitive to infrared, visible or ultraviolet radiation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02568—Chalcogenide semiconducting materials not being oxides, e.g. ternary compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02623—Liquid deposition
- H01L21/02628—Liquid deposition using solutions
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
- H01L31/0324—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIVBVI or AIIBIVCVI chalcogenide compounds, e.g. Pb Sn Te
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
- H01L31/1864—Annealing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention relates to an intermediate-infrared detector and a preparation method thereof. The intermediate-infrared detector comprises a substrate, a lead salt film and a passivation layer. The lead salt film is prepared by a selenosulfate solution, a lead acetate solution, a potassium hydroxide water solution and a soluble starch solution in the mass-volume percentage concentration ratio of 1: (0.8-3.5): (0.5-25): (0.0001-0.001) and in the size ratio of 1: (0.5-2.0): (0.5-4): (0.01-0.1). The intermediate-infrared detector improves the response rate and the signal to noise ratio, and reduces the production cost.
Description
Technical field
The invention belongs to photoelectron detector technical field is and in particular to a kind of mid-infrared detector and preparation method thereof.
Background technology
Infrared photoelectric detector is a kind of a kind of equipment receiving optical signal and being allowed to be converted to the signal of telecommunication, Infrared Detectorss
Refrigeration property Infrared Detectorss and non-refrigerated infrared detector are divided into the need of refrigeration according to its sensitive area.The former is mainly used in height
End military field, and the latter is due to eliminating refrigerating plant, and possess small volume, low in energy consumption, strong, life-span length of environmental suitability etc.
Advantage and widely apply.
Since the thirties in 20th century, the non-brake method photodetector in 1-3um and 3-5um spectral region is still with low one-tenth
Based on this vulcanized lead and lead selenide, (in the range of middle infrared spectrum, lead salt detector sensitivity, reliability are better than cadmium telluride and detect
Device, antimony arsenic indium detector).It is widely used according to the intrinsic photo-conductivity detector that the inner photoeffect of lead salt quasiconductor is prepared
Thermometric, detection, guidance, early warning, astronomical observation field.
Chemical bath deposition method prepares a kind of conventional art application that lead salt semiconductive thin film is chemical membrane, generally adopts sulfur
Urea or selenourea are generated by chemical deposition under alkaline environment with lead salt and (take charge of person of outstanding talent, prepare infrared detector photosensitive thin film
Method, China, cn 101170149a 2008-4-30；The chemical bath deposition pbse polycrystal film such as Chen Fengjin and its photoelectric properties
Pre-test [j]. infrared technique .2009), the lead salt thin film using the preparation of this method has relatively good photoelectric properties, red
Outer field of detecting is widely used.
The domestic at present performance report for lead salt detector is very few, mostly remains in development.And according to external
From the point of view of the development of nearly 30 years, mainly have two kinds of preparation methods, a kind of be exactly traditional low-cost as above chemical baths
(infrared detectors, 1984, vol.443, pages 60-94, san diego, california), through excessive
Year development, at present the company such as the U.S. calsensors detectivity of such lead salt detector can be brought up under room temperature
1×1010cm·hz1/2/ more than w；Another is exactly (the semicond. sci. technol. 11 such as Spain Zhan nurse Martin
(1996) 1740-1744) with the lead salt detector of the method for thermal evaporation preparation, its detectivity only has 1 × 109cm·hz1/2/w.
Content of the invention
It is an object of the invention to provide a kind of mid-infrared detector and preparation method thereof, it is red that preparation method of the present invention obtains
External detector reduces cost of manufacture while improving responsiveness, signal to noise ratio again.
In order to achieve the above object, the present invention adopts the following technical scheme that
The present invention provides a kind of mid-infrared detector, and including substrate, lead salt thin film and passivation layer, described lead salt thin film is by such as
Lower raw material is made: sodium thiosulfate solution, acetic acid lead solution, potassium hydroxide aqueous solution and soluble starch solution；Wherein, seleno
Metabisulfite solution, the ratio of the quality concentration of volume percent of acetic acid lead solution, potassium hydroxide aqueous solution and soluble starch solution
For 1:(0.8～3.5): (0.5～25): (0.0001～0.001)；Sodium thiosulfate solution, acetic acid lead solution, potassium hydroxide water
The volume ratio of solution and soluble starch solution is 1:(0.5～2.0): (0.5～4): (0.01～0.1).
The quality concentration of volume percent of described sodium thiosulfate solution is 2～200g/l.
Described substrate is vitreous silica, simple glass, the silicon chip of ultra-clear glasses, calcium fluoride or surface oxidation.
The preparation method of described mid-infrared detector, is made up of following steps:
(1) cleaning of substrate: clean substrate according to standard cleaning technique, high pure nitrogen dries up rear stored dry；
(2) configuration of deposition solution: under mixing speed 300～500rpm stirring, according to above-mentioned formula, lead acetate is molten
Liquid puts in potassium hydroxide aqueous solution, stirs to reaction completely, with the rate of addition of 9～12ml/min successively Deca seleno sulphuric acid
Sodium solution and soluble starch solution, obtain water white deposition solution after stirring；
(3) preparation of lead salt thin film substrate: first the deposition solution that step (2) obtains is moved in deposition vessel, deposition
It is that in 50～100 DEG C of water-baths, the substrate then obtaining step (1) is suspended on the middle part of deposition solution that container is placed in temperature, in
Mixing speed is that under 30～50rpm, stirring deposition 2.5～3h obtains lead salt thin film substrate；
(4) make annealing treatment: the lead salt thin film substrate that step (3) is obtained is placed in annealing furnace and is 300～500 DEG C in temperature
Lower annealing 30～90min；
(5) passivation protection: the lead salt thin film substrate after step (4) is annealed carries out coating film treatment；
(6) the lead salt thin film substrate after step (5) passivation protection carried out cutting, encapsulate and obtain product.
The reagent that in step (5), plated film is selected is zinc sulfide, silicon dioxide or calcium fluoride.
In step (5), plated film selects coater is thermal evaporation, magnetron sputtering or electron beam evaporation.
Step (6) encapsulation is using standard to series packaging technology.
With lead acetate for lead source in this technical scheme, sodium thiosulfate is selenium source, and potassium hydroxide is chelating agent, and solubility is formed sediment
Powder prepares lead salt thin film for buffer agent；Take different gases, different temperature in different annealing stages to prepared lead salt
Thin film carries out sensitized treatment；Lead salt thin film after sensitized treatment is carried out at plated film passivation protection by desirable effect using coater
Reason；Finally using techniques such as lead welding, epoxy sealings, film substrate is packaged.
Compared with prior art: the beneficial effect that the present invention obtains:
1. selenium source change: replace selenourea to grow lead salt thin film using stable and economic sodium thiosulfate, maintaining very
Also product cost is made to decrease while to improving product performance.
2. the selection of buffer agent: adopt soluble starch solution as buffer agent in chemical bath deposition, increased deposition
The viscosity of solution it is suppressed that the nucleation rate of lead salt, thus controlling the deposition velocity of lead salt.
3. chemical bath deposition device: the glass drying oven that film growth adopts adopts encapsulation process in chemical bath deposition, deposition
Total amount is certain during the course of the reaction for solution, it is to avoid timing adds deposition solution or this factor of water to deposition film performance and shape
Impact caused by looks is it is ensured that the collimation of different batches sample；Substrate keeps level during the course of the reaction, and substrate is same flat
Contact deposition liquid ion concentration in face is basically identical, and passes through the uniformity that stirring at low speed can improve thin film further.
4. sensitization technique: the present invention carries out sensitized treatment to lead salt thin film at different temperatures using multiple pure gases.
5. properties of product: the lead salt detector chip that the present invention prepares after plated film detectivity up to 1～3 ×
1010cm·hz1/2/ w and more than.
Brief description
Fig. 1 implements to use chemical bath deposition schematic device for the present invention；
Fig. 2 prepares film scanning electron microscopic picture for chemical bath deposition of the present invention；
Fig. 3 anneals for present invention enforcement and is sensitized schematic diagram；
Fig. 4 is coating process flow chart of the present invention；
Fig. 5 is encapsulation schematic diagram of the present invention
1 magnetic stirring apparatuss；2 mixing control systems；3 water bath devices；4 distilled water holding；5 reaction solutions；6 substrates；7
Thermometer；8 temperature-controlling systems；The adopted sealing container of 9 depositions.
Specific embodiment
Fig. 1 is chemical bath deposition device of the present invention, and substrate 6 is fixing on the securing means, then horizontally suspends molten in depositing
The middle and lower part (substrate distance deposition solution bottom, top 4cm about) of liquid 5；In deposition process, deposition solution 5 is placed in water-bath 4,
Sealing Device sealing deposition solution 5 is stable to ensure deposition solution total amount；Temperature controller 8 receives the feedback of thermometer 7, and controls
Heater processed heats up and maintains the required temperature of deposition；By adjusting mixing control device 2, the rotating speed to change stirrer makes
Deposition solution 5 concentration is consistent.
Fig. 3 prepares the sensitization apparatus of Infrared Detectorss for the present invention, adjusts temperature controller, the speed making annealing furnace to set
Rate is heated/cooled to design temperature；Regulating time controller is adjusting the sensitization time of lead salt thin film substrate；By gas flow
Adjust the required air/nitrogen/oxygen charge flow rate of sensitization.
Fig. 4 prepares the coating process of Infrared Detectorss for the present invention, lead salt thin film substrate is put into coater cavity, with covering
Lamina membranacea mask is simultaneously fixing, plates the protecting film/anti-reflection film of last layer specific thickness to play passivation using coater to photosensitive region
Protective effect.
Fig. 5 prepares the encapsulation schematic diagram of Infrared Detectorss for the present invention, using to such as dispensing, lead welding, Vacuum Package
Serial packaging technology is packaged to the lead salt thin film substrate of preparation.
With reference to embodiment to further description of the present invention, but it is not intended to limit present disclosure.
The alternative substrate of the present invention includes but is not limited to: quartz, simple glass, ultra-clear glasses, calcium fluoride, Surface Oxygen
Silicon chip changed etc..
The present invention adopts water as distilled water, and distilled water resistivity is in 15m ω cm-1More than.
The reagent that the present invention adopts includes but is not limited to: sodium thiosulfate, selenium powder, sodium sulfite, lead acetate, hydroxide
Potassium, soluble starch etc., it is pure that selected reagent purity is analysis.
Preparation of reagents
(1) the sodium thiosulfate solution of 2～200g/l is configured according to the thickness that lead selenide need to deposit.Example: 10g/l's
na2seso3Solution preparation method is as follows: 500ml selenium powder containing 2.2g and and 13.15g na2so3Distilled water solution in 90 DEG C of bars
It is heated at reflux 3 hours under part.Selenium powder and sodium sulfite reaction form colourless transparent solution in this process, and this solution is referred to as molten
Liquid 1.
(2) 3.61～360g/l acetic acid lead solution is configured according to the thickness that lead selenide need to deposit.Example: 18g/l lead acetate
Solution preparation method is as follows: 9.5g lead acetate adds in 500ml distilled water, stirs 2h, filter insoluble matter in 60 DEG C of environment,
Obtain final product, this solution abbreviation solution 2.
(3) the ph value according to needed for deposition solution and deposition velocity configuration 4～200g/l potassium hydroxide aqueous solution.Example:
2g potassium hydroxide solid is dissolved in 500ml distilled water thus preparing 4g/l potassium hydroxide solution, this solution abbreviation solution 3.
(4) the soluble starch solution of 0.1～10g/l is configured according to depositing operation.Example: 0.1g soluble starch exists
In 100ml, 50 DEG C of distilled water, stirring and dissolving configures the soluble starch solution of 1g/l, this solution abbreviation solution 4.
The cleaning of substrate in preparation method of the present invention: specifically substrate is cleaned up according to standard cleaning technique,
High pure nitrogen dries up and stores in an oven.The quartz substrate of example: 50mm × 25mm, soaks 5 min with chromic acid solution, takes out
Cleaned up with distilled water, use ethanol, acetone, distilled water to be cleaned by ultrasonic 5 min successively, high pure nitrogen is dried and stored up in an oven
Deposit.
The configuration of deposition solution: according to above-mentioned formula by the solution 2 of certain volume under the stirring of rotating speed 300～500rpm
Add in solution 3, stir to reaction completely, with the rate of addition of 9～12ml/min successively Deca solution 1 and solution 4, stir
Water white deposition solution is obtained after uniformly.Example: 1. 80ml solution 3 adds into filling 420ml resistivity 15m ω cm-1
The glass container of distilled water in, under stirring, 50ml solution 1 is added with the rate of addition of 9ml/min, stirring 10min guarantees no white
Color floccule generates；2. with the rate of addition Deca 5ml solution 4 of 9ml/min and 50ml solution 1, continue to stir after being added dropwise to complete
Mix 10min and obtain water white deposition solution, this solution abbreviation solution 5.
The preparation of lead salt thin film substrate: first deposition solution is moved in deposition vessel, it is 50 that deposition vessel is placed in temperature
In～100 DEG C of water-baths, then the substrate cleaning up is suspended on the middle part of deposition solution, is to stir under 30～50rpm in rotating speed
Mix deposition 2.5～3h and obtain lead salt thin film substrate；Example: 1. open magnetic stirring apparatuss, adjust and control bath temperature to 80
℃；2. it is transferred to quantitative for the solution preparing 5 in 500ml glass deposition vessel, by cleaned quartz substrate horizontal positioned
In deposition solution；3. sealing is contained with the glass deposition vessel of solution 5；Deposition vessel is placed in water-bath and heats and adjust
Magnetic stirring apparatuss rotating speed 50rpm, starts deposition process；4. terminate after 3h to deposit and take out substrate.
Sensitized treatment: the lead salt thin film that chemical bath deposition is prepared is placed in annealing furnace, under the conditions of 300～500 DEG C,
It is passed through 10～20ml/min cm2Nitrogen or oxygen or air, continue 60～90min.
Passivation protection: using thermal evaporation or magnetron sputtering or electron beam evaporation deposition machine to the lead salt thin film substrate after sensitization
Plate certain thickness zinc sulfide or silicon dioxide or calcium fluoride.
Encapsulation: lead salt thin film substrate is packaged according to series packaging technology.
In contrast, the technique of physical method prepare complex: 1. high-resistance silicon chip does surface oxidation treatment, dioxy
The thickness of SiClx oxide layer is more than 700nm；2. gold-plated electrode pattern required for being made using photoetching process simultaneously secondary is lithographically
Evaporated film is prepared；3. deposit 1.5um polycrystalline lead selenide on the silicon chip after thermal oxidation for the method utilizing thermal evaporation
Thin film；4., after removing photoresist, thin film is carried out with sensitization annealing；5. do passivation protection to the thin film after processing to process；
6. photoetching corrode silicon dioxide, gold-plated conductive layer windowing；7. lead packages.At present, physical preparation method is prepared lead salt and is visited
The detectivity surveying device is 1 × 109cm·hz1/2/ w, is weaker than chemical deposition；Electricity refrigeration is needed to a certain extent during use
The serviceability to improve product for the intervention of technology, technique preparation and complexity determine the input of its high cost.
Example one:
Select one 30 × 40mm quartz substrate, standard cleaning technique cleans up, high pure nitrogen is dried and is placed in fixed support
On.
100ml mass concentration is that the potassium hydroxide aqueous solution of 120g/l adds into the glass container filling 190ml distilled water
In, low whipping speed be 300rpm in the case of be slowly added to 100ml mass concentration be 180g/l acetic acid lead solution, after 10min
The soluble starch solution as 1g/l for the 10ml mass concentration, 100ml mass concentration are sequentially added with the rate of addition of 10ml/min
Sodium thiosulfate solution for 100g/l, obtains the water white deposition solution of 500ml after stirring 10min.
As shown in figure 1, horizontally suspending the fixed support with substrate in deposition solution, and transfer to 75 DEG C, 40rpm
In the water-bath of rotating speed, sealing, take out substrate after 3h and terminate to deposit, the lead salt thin film of chemical bath deposition preparation is as shown in Figure 2.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 400 DEG C with 20 DEG C/min heating rate；It is passed through 10ml/min cm to annealing furnace2Oxygen, keeps
50min；Annealing furnace is cooled to 320 DEG C with 20 DEG C/min speed, keeps 30min；In 10ml/min cm2Nitrogen protection is lower to anneal
Stove is cooled to room temperature, terminates to anneal and take out film substrate, specific sensitization apparatus are as shown in Figure 3.
As described in Figure 4, lead salt thin film substrate is put into coater cavity, with earth silicon mask plate mask and fixing, magnetic
Control sputter coating machine plates the silicon dioxide of last layer 800nm to photosensitive region；Take out substrate, change gold mast plate mask and fix,
Put into cavity, then electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 1.2um can be prepared by this method, particle size is the lead salt thin film of 900nm, resistance after sensitization
Detectivity 1.5 × 10 can be prepared after 1.5m ω/, passivation protection10cm·hz1/2The sample of/w.
Example two:
Select one 30 × 40mm common glass substrate, standard cleaning technique cleans up, high pure nitrogen is dried and is placed in fixing
On support.
Measure the sodium thiosulfate solution for 205g/l for the 100ml mass concentration successively, 100ml mass concentration is 180g/l's
The solubility that acetic acid lead solution, 100ml mass concentration are the potassium hydroxide aqueous solution of 160g/l, 10ml mass concentration is 1g/l is formed sediment
Powder solution, 190ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 80 DEG C, the water-bath of 45rpm rotating speed
In, sealing, take out substrate after 2.5h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 400 DEG C with 40 DEG C/min heating rate；It is passed through 10ml/min cm to annealing furnace2Oxygen, keeps 1h,
Annealing furnace is cooled to 320 DEG C with 20 DEG C/min speed, keeps 30min；In 10ml/min cm2The lower annealing furnace cooling of nitrogen protection
To room temperature, terminate to anneal and take out film substrate.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 1um can be prepared by this method, particle size is the lead salt thin film of 1000nm, resistance 1.4m after sensitization
It is 9 × 10 that ω/, non-passivation protection prepare sample detectivity9cm·hz1/2/w.
Example three:
Select one 30 × 40mm ultra-clear glasses substrate, standard cleaning technique cleans up, high pure nitrogen is dried and is placed in fixing
On support.
Measure the sodium thiosulfate solution for 20g/l for the 50ml mass concentration successively, 50ml mass concentration is the acetic acid of 36g/l
Lead solution, 50ml mass concentration are the potassium hydroxide aqueous solution of 80g/l, the soluble starch for 0.1g/l for the 1ml mass concentration is molten
Liquid, 350ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 90 DEG C, the water-bath of 50rpm rotating speed
In, sealing, take out substrate after 3h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 4mm × 3mm.
Lead salt thin film substrate is put into coater cavity, with earth silicon mask plate mask and fixing, magnetron sputtering plating
Machine plates the silicon dioxide of last layer 600nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, so
Afterwards electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-8 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is 3mm × 3mm3
× 3 Infrared Detectorss.
Thickness 0.9um can be prepared by this method, particle size is the lead salt thin film of 1000nm, at sensitization
Reason, the no obvious photoelectric properties of the sample prepared.
Example four:
Select one 30 × 40mm quartz substrate, standard cleaning technique cleans up, high pure nitrogen is dried and is placed in fixed support
On.
Measure the sodium thiosulfate solution for 100g/l for the 60ml mass concentration successively, 60ml mass concentration is the vinegar of 180g/l
Lead plumbate solution, 100ml mass concentration are the potassium hydroxide aqueous solution of 80g/l, the soluble starch for 1g/l for the 1ml mass concentration is molten
Liquid, 280ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 60 DEG C, the water-bath of 35rpm rotating speed
In, sealing, take out substrate after 3h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 400 DEG C with 20 DEG C/min heating rate；It is passed through 20ml/min cm to annealing furnace2Oxygen, keeps
30min, annealing furnace is cooled to 320 DEG C with 20 DEG C/min speed, keeps 30min；In 10ml/min cm2Nitrogen protection is lower to anneal
Stove is cooled to room temperature, terminates to anneal and take out film substrate.
Lead salt thin film substrate is put into coater cavity, with calcium fluoride mask plate mask and fixing, electron beam evaporation deposition
Machine plates the calcium fluoride of last layer 200nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, then
Electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 0.8um can be prepared by this method, particle size is the lead salt thin film of 800nm, resistance after sensitization
Detectivity 1.2 × 10 can be prepared after 1.5m ω/, passivation protection10cm·hz1/2The sample of/w.
Example five:
" quartz substrate, standard cleaning technique cleans up, and high pure nitrogen is dried and is placed on fixed support to select 1.
Measuring 50ml mass concentration successively is the sodium thiosulfate solution of 100g/l, the acetic acid of 50ml mass concentration 360g/l
Lead solution, the potassium hydroxide aqueous solution of 160ml mass concentration 80g/l, the soluble starch solution of 1ml mass concentration 1g/l,
240ml distilled water configures 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 75 DEG C, the water-bath of 40rpm rotating speed
In, sealing, take out substrate after 3 and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 500 DEG C with 40 DEG C/min heating rate；It is passed through 10ml/min cm to annealing furnace2Oxygen, keeps
20min, annealing furnace is cooled to 350 DEG C with 20 DEG C/min speed, keeps 15min；In 10ml/min cm2Nitrogen protection is lower to anneal
Stove is cooled to room temperature, terminates to anneal and take out film substrate.
Lead salt thin film substrate is put into coater cavity, with zinc sulfide mask plate mask and fixing, using thermal evaporation plated film
Machine plates the zinc sulfide of last layer 400nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, then
Electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 1.3um can be prepared by this method, particle size is the lead salt thin film of 1100nm, 8m after sensitized treatment
Detectivity 1 × 10 can be prepared after ω/, passivation protection9cm·hz1/2The sample of/w.
Example six:
" surface oxidation silicon chip substrate, standard cleaning technique cleans up, and high pure nitrogen is dried and is placed in fixing to select 1
On frame.
Measure the sodium thiosulfate solution for 100g/l for the 100ml mass concentration successively, 100ml mass concentration is 180g/l's
The solubility that acetic acid lead solution, 100ml mass concentration are the potassium hydroxide aqueous solution of 120g/l, 10ml mass concentration is 1g/l is formed sediment
Powder solution, 190ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 65 DEG C, the water-bath of 35rpm rotating speed
In, sealing, take out substrate after 2.5h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 450 DEG C with 30 DEG C/min heating rate；It is passed through 10ml/min cm to annealing furnace2Oxygen, keeps
40min, annealing furnace is cooled to 320 DEG C with 20 DEG C/min speed, keeps 30min；In 10ml/min cm2Nitrogen protection is lower to anneal
Stove is cooled to room temperature, terminates to anneal and take out film substrate.
Lead salt thin film substrate is put into coater cavity, with earth silicon mask plate mask and fixing, magnetron sputtering plating
Machine plates the silicon dioxide of last layer 800nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, so
Afterwards electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 1.1um can be prepared by this method, particle size is the lead salt thin film of 900nm, resistance after sensitization
Detectivity 7 × 10 can be prepared after 4.5m ω/, passivation protection9cm·hz1/2The sample of/w.
Example seven:
" ultra-clear glasses substrate, standard cleaning technique cleans up, and high pure nitrogen is dried and is placed on fixed support to select 1.
Measure the sodium thiosulfate solution for 100g/l for the 60ml mass concentration successively, 60ml mass concentration is the vinegar of 180g/l
Lead plumbate solution, 100ml mass concentration are the potassium hydroxide aqueous solution of 80g/l, the soluble starch for 1g/l for the 1ml mass concentration is molten
Liquid, 280ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 80 DEG C, the water-bath of 40rpm rotating speed
In, sealing, take out substrate after 2.5h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 350 DEG C with 10 DEG C/min heating rate；It is passed through 10ml/min cm to annealing furnace2Oxygen, keeps 1h,
Annealing furnace is cooled to 300 DEG C with 10 DEG C/min speed, keeps 30min；In 10ml/min cm2The lower annealing furnace cooling of nitrogen protection
To room temperature, terminate to anneal and take out film substrate.
Lead salt thin film substrate is put into coater cavity, with zinc sulfide mask plate mask and fixing, thermal evaporation coater pair
Photosensitive region plates the zinc sulfide of last layer 400nm；Take out substrate, change gold mast plate mask and fix, put into cavity, then to electricity
Polar region domain carries out thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 0.9um can be prepared by this method, particle size is the lead salt thin film of 800nm, and resistance after being sensitized
Detectivity 1 × 10 can be prepared after 0.3m ω/, passivation protection9cm·hz1/2The sample of/w.
Example eight:
Select one 25 × 50mm quartz substrate, standard cleaning technique cleans up, high pure nitrogen is dried and is placed in fixed support
On.
Measure the sodium thiosulfate solution for 100g/l for the 100ml mass concentration successively, 100ml mass concentration is 180g/l's
The solubility that acetic acid lead solution, 100ml mass concentration are the potassium hydroxide aqueous solution of 120g/l, 10ml mass concentration is 1g/l is formed sediment
Powder solution, 190ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 55 DEG C, the water-bath of 30rpm rotating speed
In, sealing, take out substrate after 3h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；It is being passed through 10ml/min cm2
Under condition of nitrogen gas, annealing furnace rises to 450 DEG C with 20 DEG C/min heating rate and maintains 1h；It is being passed through 10ml/min cm2Nitrogen bar
It is cooled to room temperature under part, take out substrate and terminate to be sensitized.
Lead salt thin film substrate is put into coater cavity, with earth silicon mask plate mask and fixing, magnetron sputtering plating
Machine plates the silicon dioxide of last layer 800nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, so
Afterwards electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 0.9um can be prepared by this method, particle size is the lead salt thin film of 1000nm, resistance after sensitization
Detectivity 1 × 10 can be prepared after 0.05m ω/, passivation protection9cm·hz1/2The sample of/w.
Example nine:
Select one 25 × 50mm common glass substrate, standard cleaning technique cleans up, high pure nitrogen is dried and is placed in fixing
On support.
Measure the sodium thiosulfate solution for 20g/l for the 50ml mass concentration successively, 50ml mass concentration is the acetic acid of 36g/l
Lead solution, 50ml mass concentration are the potassium hydroxide aqueous solution of 80g/l, the soluble starch for 0.1g/l for the 1ml mass concentration is molten
Liquid, 350ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 65 DEG C, the water-bath of 35rpm rotating speed
In, sealing, take out substrate after 3h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 370 DEG C with 20 DEG C/min heating rate；It is passed through 15ml/min cm to annealing furnace2Oxygen, keeps
45min, annealing furnace is cooled to 300 DEG C with 10 DEG C/min speed, keeps 30min；In 10ml/min cm2Nitrogen protection is lower to anneal
Stove is cooled to room temperature, terminates to anneal and take out film substrate.
Lead salt thin film substrate is put into coater cavity, with calcium fluoride mask plate mask and fixing, electron beam evaporation deposition
Machine plates the calcium fluoride of last layer 200nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, then
Electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 1.2um can be prepared by this method, particle size is the lead salt thin film of 1000nm, resistance after sensitization
Detectivity 1.3 × 10 can be prepared after 1.1m ω/, passivation protection10cm·hz1/2The sample of/w.
Example ten:
" calcium fluoride substrate, standard cleaning technique cleans up, and high pure nitrogen is dried and is placed on fixed support to select 1.
Measure the sodium thiosulfate solution for 100g/l for the 60ml mass concentration successively, 60ml mass concentration is the vinegar of 180g/l
Lead plumbate solution, 100ml mass concentration are the potassium hydroxide aqueous solution of 80g/l, the soluble starch for 1g/l for the 1ml mass concentration is molten
Liquid, 280ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 60 DEG C, the water-bath of 40rpm rotating speed
In, sealing, take out substrate after 3h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；It is being passed through 10ml/min cm2
Under Oxygen Condition, annealing furnace rises to 400 DEG C with 40 DEG C/min heating rate and maintains 1h；It is being passed through 10ml/min cm2Oxygen bar
It is cooled to room temperature under part, take out substrate and terminate to be sensitized.
Lead salt thin film substrate is put into coater cavity, with earth silicon mask plate mask and fixing, magnetron sputtering plating
Machine plates the silicon dioxide of last layer 500nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, so
Afterwards electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 0.8um can be prepared by this method, particle size is the lead salt thin film of 800nm, resistance 4m after sensitization
Detectivity 4 × 10 can be prepared after ω/, passivation protection9cm·hz1/2The sample of/w.
Example 11:
Select one 25 × 50mm ultra-clear glasses substrate, standard cleaning technique cleans up, high pure nitrogen is dried and is placed in fixing
On support.
Measure the sodium thiosulfate solution for 100g/l for the 100ml mass concentration successively, 100ml mass concentration is the l of 180g/
The solubility that acetic acid lead solution, 100ml mass concentration are the potassium hydroxide aqueous solution of 120g/l, 10ml mass concentration is 1g/l is formed sediment
Powder solution, 190ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 80 DEG C, the water-bath of 40rpm rotating speed
In, sealing, take out substrate after 3h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 360 DEG C with 20 DEG C/min heating rate；It is passed through 10ml/min cm to annealing furnace2Air, keeps 1h,
Annealing furnace is cooled to 300 DEG C with 10 DEG C/min speed, keeps 30min；In 10ml/min cm2The lower annealing furnace cooling of nitrogen protection
To room temperature, terminate to anneal and take out film substrate.
Lead salt thin film substrate is put into coater cavity, with calcium fluoride mask plate mask and fixing, electron beam evaporation deposition
Machine plates the calcium fluoride of last layer 150nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, then
Electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 1.3um can be prepared by this method, particle size is the lead salt thin film of 1000nm, resistance after sensitization
Detectivity 1.7 × 10 can be prepared after 0.8m ω/, passivation protection10cm·hz1/2The sample of/w.
Example 12:
" surface oxidation silicon chip substrate, standard cleaning technique cleans up, and high pure nitrogen is dried and is placed in fixing to select 1
On frame.
Measuring 50ml mass concentration successively is the sodium thiosulfate solution of 100g/l, the acetic acid of 50ml mass concentration 360g/l
Lead solution, the potassium hydroxide aqueous solution of 160ml mass concentration 80g/l, the soluble starch solution of 1ml mass concentration 1g/l,
240ml distilled water configures 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 50 DEG C, the water-bath of 30rpm rotating speed
In, sealing, take out substrate after 3h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；It is being passed through 10ml/min cm2
Under air conditionses, annealing furnace rises to 450 DEG C with 20 DEG C/min heating rate and maintains 40min；It is being passed through 10ml/min cm2Air
Under the conditions of be cooled to room temperature, take out substrate and terminate to be sensitized.
Lead salt thin film substrate is put into coater cavity, with zinc sulfide mask plate mask and fixing, thermal evaporation coater pair
Photosensitive region plates the zinc sulfide of last layer 400nm；Take out substrate, change gold mast plate mask and fix, put into cavity, then to electricity
Polar region domain carries out thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 0.7um can be prepared by this method, particle size is the lead salt thin film of 600nm, resistance after sensitization
Detectivity 1 × 10 can be prepared after 0.2m ω/, passivation protection9cm·hz1/2The sample of/w.
Example 13:
" quartz substrate, standard cleaning technique cleans up, and high pure nitrogen is dried and is placed on fixed support to select 1.
Measure the sodium thiosulfate solution for 100g/l for the 100ml mass concentration successively, 100ml mass concentration is 180g/l's
The solubility that acetic acid lead solution, 100ml mass concentration are the potassium hydroxide aqueous solution of 120g/l, 10ml mass concentration is 1g/l is formed sediment
Powder solution, 190ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 75 DEG C, the water-bath of 40rpm rotating speed
In, sealing, take out substrate after 2.5h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 400 DEG C with 20 DEG C/min heating rate；It is passed through 10ml/min cm to annealing furnace2Air, keeps
40min, annealing furnace is cooled to 350 DEG C with 20 DEG C/min speed, keeps 10min；In 10ml/min cm2Nitrogen protection is lower to anneal
Stove is cooled to room temperature, terminates to anneal and take out film substrate.
Lead salt thin film substrate is put into coater cavity, with earth silicon mask plate mask and fixing, magnetron sputtering plating
Machine plates the silicon dioxide of last layer 800nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, so
Afterwards electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 1.2um can be prepared by this method, particle size is the lead salt thin film of 900nm, resistance after sensitization
Detectivity 2 × 10 can be prepared after 0.2m ω/, passivation protection9cm·hz1/2The sample of/w.
Example 14:
Select one 30 × 40mm common glass substrate, standard cleaning technique cleans up, high pure nitrogen is dried and is placed in fixing
On support.
Measure the sodium thiosulfate solution for 20g/l for the 50ml mass concentration successively, 50ml mass concentration is the acetic acid of 36g/l
Lead solution, 50ml mass concentration are the potassium hydroxide aqueous solution of 80g/l, the soluble starch for 0.1g/l for the 1ml mass concentration is molten
Liquid, 350ml distilled water configure 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 80 DEG C, the water-bath of 35rpm rotating speed
In, sealing, take out substrate after 3h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 450 DEG C with 20 DEG C/min heating rate；It is passed through 12ml/min cm to annealing furnace2Oxygen, keeps
45min, annealing furnace is cooled to 320 DEG C with 10 DEG C/min speed, keeps 30min；In 10ml/min cm2Nitrogen protection is lower to anneal
Stove is cooled to room temperature, terminates to anneal and take out film substrate.
Lead salt thin film substrate is put into coater cavity, with zinc sulfide mask plate mask and fixing, using thermal evaporation plated film
Machine plates the zinc sulfide of last layer 400nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, then
Electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 1.3um can be prepared by this method, particle size is the lead salt thin film of 1000nm, resistance after sensitization
Detectivity 1.2 × 10 can be prepared after 1.4m ω/, passivation protection10cm·hz1/2The sample of/w.
Example 15:
Select one 30 × 40mm quartz substrate, standard cleaning technique cleans up, high pure nitrogen is dried and is placed in fixed support
On.
Measuring 50ml mass concentration successively is the sodium thiosulfate solution of 100g/l, the l acetic acid of 50ml mass concentration 360g/
Lead solution, the potassium hydroxide aqueous solution of 160ml mass concentration 80g/l, the soluble starch solution of 1ml mass concentration 1g/l,
240ml distilled water configures 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 70 DEG C, the water-bath of 40rpm rotating speed
In, sealing, take out substrate after 3h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 400 DEG C with 40 DEG C/min heating rate；It is passed through 15ml/min cm to annealing furnace2Oxygen, keeps
30min, annealing furnace is cooled to 320 DEG C with 10 DEG C/min speed, keeps 10min；In 10ml/min cm2Nitrogen protection is lower to anneal
Stove is cooled to room temperature, terminates to anneal and take out film substrate.
Lead salt thin film substrate is put into coater cavity, with earth silicon mask plate mask and fixing, magnetron sputtering plating
Machine plates the silicon dioxide of last layer 800nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, so
Afterwards electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 1.2um can be prepared by this method, particle size is the lead salt thin film of 900nm, resistance after sensitization
Detectivity 1.4 × 10 can be prepared after 1.9m ω/, passivation protection10cm·hz1/2The sample of/w.
Example 16:
" ultra-clear glasses substrate, standard cleaning technique cleans up, and high pure nitrogen is dried and is placed on fixed support to select 1.
Measuring 50ml mass concentration successively is the sodium thiosulfate solution of 100g/l, the acetic acid of 50ml mass concentration 360g/l
Lead solution, the potassium hydroxide aqueous solution of 160ml mass concentration 80g/l, the soluble starch solution of 1ml mass concentration 1g/l,
240ml distilled water configures 500ml deposition solution according to the mode of example 1.
Fixed support with substrate horizontally suspends in deposition solution, and transfers to 80 DEG C, the water-bath of 35rpm rotating speed
In, sealing, take out substrate after 2.5h and terminate to deposit.
Attachment on substrate is cleaned up, and is cut to the film substrate of 3mm × 2mm.
Film substrate is put into annealing furnace, checks and guarantee that annealing device air-tightness is good；In 10ml/min cm2Nitrogen
The lower annealing furnace of protection rises to 350 DEG C with 20 DEG C/min heating rate；It is passed through 15ml/min cm to annealing furnace2Oxygen, keeps 1h,
Annealing furnace is cooled to 300 DEG C with 10 DEG C/min speed, keeps 30min；In 10ml/min cm2The lower annealing furnace cooling of nitrogen protection
To room temperature, terminate to anneal and take out film substrate.
Lead salt thin film substrate is put into coater cavity, with earth silicon mask plate mask and fixing, magnetron sputtering plating
Machine plates the silicon dioxide of last layer 800nm to photosensitive region；Take out substrate, change gold mast plate mask and fix, put into cavity, so
Afterwards electrode zone is carried out with thermal resistance evaporation and plates one layer of 300nm gold film electrode.
Using to-5 packaging technology, lead salt thin film substrate is packaged, thus preparing photosensitive area is that 2mm × 2mm is red
External detector.
Thickness 0.9um can be prepared by this method, particle size is the lead salt thin film of 900nm, resistance after sensitization
Detectivity 5 × 10 can be prepared after 1.0m ω/, passivation protection9cm·hz1/2The sample of/w.
Above-described is only the preferred embodiment of the present invention it is noted that for a person skilled in the art,
Under the premise of without departing from general idea of the present invention, some changes and improvements can also be made, these also should be considered as the present invention's
Protection domain.
Claims (7)
1. a kind of mid-infrared detector, including substrate, lead salt thin film and passivation layer it is characterised in that: described lead salt thin film is by such as
Lower raw material is made: sodium thiosulfate solution, acetic acid lead solution, potassium hydroxide aqueous solution and soluble starch solution；Wherein, seleno
Metabisulfite solution, the ratio of the quality concentration of volume percent of acetic acid lead solution, potassium hydroxide aqueous solution and soluble starch solution
For 1:(0.8～3.5): (0.5～25): (0.0001～0.001)；Sodium thiosulfate solution, acetic acid lead solution, potassium hydroxide water
The volume ratio of solution and soluble starch solution is 1:(0.5～2.0): (0.5～4): (0.01～0.1).
2. mid-infrared detector according to claim 1 it is characterised in that: the quality volume of described sodium thiosulfate solution
Percent concentration is 2～200g/l.
3. mid-infrared detector according to claim 1 it is characterised in that: described substrate be quartz, simple glass, ultrawhite
The silicon chip of glass, calcium fluoride or surface oxidation.
4. the method preparing mid-infrared detector according to claim 1 is it is characterised in that be made up of following steps:
(1) cleaning of substrate: substrate is cleaned up according to standard cleaning technique, high pure nitrogen dries up rear stored dry；
(2) configuration of deposition solution: under mixing speed 300～500rpm stirring, according to above-mentioned formula, acetic acid lead solution is thrown
Enter in potassium hydroxide aqueous solution, stir to reaction completely, molten with the rate of addition of 9～12ml/min successively Deca sodium thiosulfate
Liquid and soluble starch solution, obtain water white deposition solution after stirring；
(3) preparation of lead salt thin film substrate: first the deposition solution that step (2) obtains is moved in deposition vessel, deposition vessel
Being placed in temperature is that in 50～100 DEG C of water-baths, the substrate then obtaining step (1) is suspended on the middle part of deposition solution, in stirring
Speed is that under 30～50rpm, stirring deposition 2.5～3h obtains lead salt thin film substrate；
(4) make annealing treatment: the lead salt thin film substrate that step (3) is obtained is placed in annealing furnace and moves back at temperature is 300～500 DEG C
Fire processes 30～90min；
(5) passivation protection: the lead salt thin film substrate after step (4) is annealed carries out coating film treatment；
(6) the lead salt thin film substrate after step (5) passivation protection carried out cutting, encapsulate and obtain product.
5. according to claim 4 preparation mid-infrared detector preparation method it is characterised in that: plated film in step (5)
From reagent be zinc sulfide, silicon dioxide or calcium fluoride.
6. according to claim 4 preparation mid-infrared detector preparation method it is characterised in that: plated film in step (5)
From coater be thermal evaporation, magnetron sputtering or electron beam evaporation.
7. according to claim 4 preparation mid-infrared detector preparation method it is characterised in that: step (6) encapsulation adopt
With standard to series packaging technology.
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| CN109721036A (en) * | 2019-01-02 | 2019-05-07 | 北京科技大学 | A kind of method of chemical liquid phase reaction preparation selenizing thin film lead |
| CN110299430B (en) * | 2019-06-06 | 2022-11-11 | 华中科技大学 | Semiconductor thin film photoelectric detector and preparation method thereof |
| CN113345972B (en) * | 2021-03-22 | 2024-05-14 | 江苏大学 | Layered polycrystalline lead selenide photoelectric film and preparation method thereof |
| CN114883431A (en) * | 2022-05-31 | 2022-08-09 | 中国科学院重庆绿色智能技术研究院 | Ultraviolet/infrared dual-band photoelectric detector and preparation method thereof |
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Effective date of registration: 20190523 Address after: 459000 High-tech Industrial Agglomeration Zone in Jiyuan City, Henan Province Patentee after: Jiyuan Aitan Electronic Technology Co., Ltd. Address before: 459000 Xiangyuan District, Binhan Road, Jiyuan City, Henan Province Patentee before: Yuan Zijian |