CN109273355A - A kind of selenium cell preparation process - Google Patents
A kind of selenium cell preparation process Download PDFInfo
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- CN109273355A CN109273355A CN201810626521.6A CN201810626521A CN109273355A CN 109273355 A CN109273355 A CN 109273355A CN 201810626521 A CN201810626521 A CN 201810626521A CN 109273355 A CN109273355 A CN 109273355A
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 252
- 239000011669 selenium Substances 0.000 title claims abstract description 244
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 242
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 77
- 238000001704 evaporation Methods 0.000 claims abstract description 42
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 40
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 40
- 230000008020 evaporation Effects 0.000 claims abstract description 39
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 33
- 239000000956 alloy Substances 0.000 claims abstract description 33
- 238000003860 storage Methods 0.000 claims abstract description 27
- 239000007921 spray Substances 0.000 claims abstract description 24
- 238000005488 sandblasting Methods 0.000 claims abstract description 20
- 238000004080 punching Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000007689 inspection Methods 0.000 claims abstract description 15
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010931 gold Substances 0.000 claims abstract description 9
- 229910052737 gold Inorganic materials 0.000 claims abstract description 9
- 230000004927 fusion Effects 0.000 claims abstract description 7
- 238000004806 packaging method and process Methods 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 74
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 74
- 239000004411 aluminium Substances 0.000 claims description 62
- 238000010438 heat treatment Methods 0.000 claims description 45
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 36
- 238000012360 testing method Methods 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 27
- 238000005259 measurement Methods 0.000 claims description 19
- 238000007792 addition Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 14
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- 230000001105 regulatory effect Effects 0.000 claims description 12
- 229910052718 tin Inorganic materials 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 11
- XGGLLRJQCZROSE-UHFFFAOYSA-K ammonium iron(iii) sulfate Chemical compound [NH4+].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGGLLRJQCZROSE-UHFFFAOYSA-K 0.000 claims description 10
- 238000004090 dissolution Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 9
- 229910052793 cadmium Inorganic materials 0.000 claims description 9
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 9
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 9
- 229910052753 mercury Inorganic materials 0.000 claims description 9
- 229910052716 thallium Inorganic materials 0.000 claims description 9
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 claims description 9
- NJYFRQQXXXRJHK-UHFFFAOYSA-N (4-aminophenyl) thiocyanate Chemical compound NC1=CC=C(SC#N)C=C1 NJYFRQQXXXRJHK-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000009792 diffusion process Methods 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 8
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 claims description 6
- 229910000838 Al alloy Inorganic materials 0.000 claims description 6
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003990 capacitor Substances 0.000 claims description 6
- 239000000498 cooling water Substances 0.000 claims description 6
- 229920001971 elastomer Polymers 0.000 claims description 6
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000010008 shearing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000012797 qualification Methods 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 238000004448 titration Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 4
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 4
- 238000005485 electric heating Methods 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- CXMYWOCYTPKBPP-UHFFFAOYSA-N 3-(3-hydroxypropylamino)propan-1-ol Chemical compound OCCCNCCCO CXMYWOCYTPKBPP-UHFFFAOYSA-N 0.000 claims description 3
- 229920000742 Cotton Polymers 0.000 claims description 3
- 239000006004 Quartz sand Substances 0.000 claims description 3
- CSBHIHQQSASAFO-UHFFFAOYSA-N [Cd].[Sn] Chemical compound [Cd].[Sn] CSBHIHQQSASAFO-UHFFFAOYSA-N 0.000 claims description 3
- 238000003556 assay Methods 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000012937 correction Methods 0.000 claims description 3
- 230000007547 defect Effects 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000009863 impact test Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000005580 one pot reaction Methods 0.000 claims description 3
- 239000012716 precipitator Substances 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 229910002058 ternary alloy Inorganic materials 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- 230000009466 transformation Effects 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- 235000007466 Corylus avellana Nutrition 0.000 claims description 2
- 240000003211 Corylus maxima Species 0.000 claims description 2
- GLVPUAWFPNGKHO-UHFFFAOYSA-L N.[Fe+2].[O-]S([O-])(=O)=O Chemical compound N.[Fe+2].[O-]S([O-])(=O)=O GLVPUAWFPNGKHO-UHFFFAOYSA-L 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 150000003342 selenium Chemical class 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000008399 tap water Substances 0.000 claims description 2
- 235000020679 tap water Nutrition 0.000 claims description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims 1
- 229910000925 Cd alloy Inorganic materials 0.000 claims 1
- 229910052794 bromium Inorganic materials 0.000 claims 1
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 239000003814 drug Substances 0.000 claims 1
- 229940079593 drug Drugs 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 206010034960 Photophobia Diseases 0.000 description 1
- RFUAMROIJXRZGD-UHFFFAOYSA-N [Br].[Se] Chemical compound [Br].[Se] RFUAMROIJXRZGD-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 208000013469 light sensitivity Diseases 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 108091008695 photoreceptors Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/06—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising selenium or tellurium in uncombined form other than as impurities in semiconductor bodies of other materials
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/06—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising selenium or tellurium in uncombined form other than as impurities in semiconductor bodies of other materials
- H01L21/10—Preliminary treatment of the selenium or tellurium, its application to the foundation plate, or the subsequent treatment of the combination
- H01L21/101—Application of the selenium or tellurium to the foundation plate
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of selenium cell preparation processes.Its selenium cell is by being sliced, developing a film, sandblasting, drying, evaporation bismuth, selenium preparation, evaporation selenium, returns and steam piece, energize in advance, punching, fusion gold, spray alloy, connection piece, main energize, chamfering, impact, electrical reset, impact, sieve, reverse measuremenet, at inspection packaging and be put in storage storage process and be prepared.Since the present invention is using semiconductor selenium as main material, selenium is formed selenium chip semiconductor element, enhance rectification and overload protection, extend the semiconductor element service life, to achieve the purpose that energy-saving coated on commutator segment using special process process.
Description
Technical field:
The present invention relates to a kind of selenium cells for being widely used in the rectification of industrial electronic electrical system and overload protection to prepare work
Skill.
Background technique:
Selenium has light sensitivity and semiconductive, is often used to manufacture photocell, photoreceptor, laser in the electronics industry
Part, infrared controller, photoelectric tube, photo resistance, optical instrument, photometer, rectifier etc..Application of the selenium in electronics industry
Account for about the 30% of aggregate demand.The important feature of selenium is that have typical semiconductor property, can be used for the detection of radio wave and whole
Stream, seletron have the features such as load resistance, high temperature resistant, electrical stability is good.
Selenium cell is the core part of selenium pile, surge absorber, semiconductor rectifier cell, and function, performance depend on
Raw material quality and technique preparation process.And commutator segment adds selenium technique preparation process also very immature at present, and selenium is coated in
Technique is too simple on commutator segment, thus causes semiconductor element rectification and overload protection too low, so as to shorten semiconductor element
The part service life.
Summary of the invention:
Technical problem to be solved by the invention is to provide using semiconductor selenium as main material, using special process
Selenium coated on commutator segment, is formed selenium chip semiconductor element, enhances rectification and overload protection, extend semiconductor element by process
The part service life reaches a kind of energy-saving selenium cell preparation process.
The technical proposal for solving the technical problem of the invention is: a kind of selenium cell of selenium cell preparation process is
By being sliced, developing a film, sandblasting, drying, evaporation bismuth, selenium preparation, evaporation selenium, time steaming piece, energize in advance, punching, fusion gold, spray conjunction
Golden, connection piece, master energize, chamfering, impact, electrical reset, impact, sieve, reverse measuremenet, pack and be put in storage storage process preparation at inspection
It forms, concrete technology preparation process are as follows:
(1) slice described in: being that an aluminium sheet greatly is cut into 0.8mm × 1015mm × 2040mm size, tight during blank
Prohibit scratch surface, surface of aluminum plate has oxide layer that can not shear, and big aluminium sheet can not be sheared before shearing if any mechanical hard defects；
(2) developing a film described in: cleaning surface of aluminum plate greasy dirt with gasoline first, then cleans surface of aluminum plate oil again with buck
Dirt, the surface of aluminum plate cleaned answer light, without foul, aluminium sheet abraded area >=10mm2, should reject, not allow flow into lower road work
Sequence；
(3) sandblasting described in: its operating process are as follows: connection precipitator power supplies first pour into quartz sand in cabin, every shift
Add sand 60kg, 4 additions should be divided within full class's working time, about 15kg, must not once pour into, then check nozzle, connect every time
Again by stable gas pressure within the scope of 68.647~88.620KPa, i.e., logical sand-blasting machine linkage mechanism power supply opens compressed air valve
It can sandblasting；Aluminium sheet after sandblasting imports sandblasting wheel and removes again, finally identifies surface, should be light grey after aluminium sheet sandblasting, surface is not
Must there are serious black trace and luminous point, need 39.227~88.260KPa air pressure to respray once if any light；
(4) drying described in: its operating process are as follows: aluminium sheet is loaded vertically into drying vehicle, master switch is opened and opens air blast
Machine is connected heating 12KW and is all switched.Drying vehicle equipped with aluminium sheet is promoted in furnace, stove first preheats before working, fire door is shut,
Furnace temperature is heated to 175 ± 5 DEG C in 15 minutes, keeps the temperature 2h, after reaching temperature, is suitably heated with 4KW or 2KW, constant temperature is carried out, is dried
After dry, heater switch is disconnected, closes air blower, disconnects master switch, pulls out load vehicle；The aluminium sheet natural cooling 10 dried~
15 minutes, be put into load vehicle, with evaporation bismuth interval time≤4h, should put in baker and save more than 4h, deposit the piece time be more than for 24 hours,
It should be dried 30 minutes again with 100~120 DEG C；
(5) the evaporation bismuth described in: its operating process are as follows: open bismuth pot gas valve, fall vacuum kettle, and plug safety
Pin, the frame for installing aluminium sheet≤20, is deposited in storage shelf, in addition cover board, hangs up support welding block, the small bismuth pot number of pressing is put into
In furnace, every pot of bismuth weight 45g ± 1g；
Evaporating bismuth process is to close big fore pump air inlet valve door, opens big fore pump, and opening is pre- greatly to pump logical pot valve,
It when vacuum degree reaches 2.666Pa, opens diffusion pump and leads to pot valve, close big pre- pump vacuum valve, the moment is in parallel with diffusion pump, beats
It opens and is pumped into air valve in advance greatly, close big pre- pump and cooling water, adjust aluminium sheet counter；When vacuum degree reaches 1.666Pa, bismuth is connected
Pot heater switch, heating are evaporated automatically after 15 minutes, and evaporation time is adjusted to 2~4 minutes, and according to upper one pot of bismuth layer, adjust bismuth
Pot power, record steam first, intermediate a piece of, last a piece of vacuum degree, have steamed last a piece of alarm whistle, closed report sound
Device switch, diffusion pump valve and heating power supply, three ten minutes later, opens Ventilating valve, falls vacuum kettle, disengages rotation clutch
Device removes baffle block, takes out the bismuth piece evaporated and is put into load vehicle, send selenium to evaporate after the assay was approved；Bismuth piece is stored in product
≤ 6h, interior, which does not allow to store, to be had and micro mercury vapour and various oils and volatile article, can not be caused on aluminium sheet
Scuffing, mechanical damage, greasy dirt, impression of the hand can not make aluminium sheet deformation；
(6) the selenium preparation described in: its operating process are as follows: weigh out the selenium powder of two parts of 70g in the balance, portion is poured on ground triangle
In beaker, 15ml liquid bromine is measured with graduated cylinder, is poured in conical flask, speed should slowly and constantly shake, will be another in beaker
Part 70ml selenium powder shake is slowly poured into triangular flask, is then closed the lid, and after storing 48h, can configure addition selenium；
System addition selenium, weighs up 5kg selenium, is poured into stainless steel agitated kettle, and heating fusing is stirred at 300~350 DEG C
2h is clamped equipped with selenium bromide triangular flask bottleneck with clamp, after dissolving on electric furnace, is poured into stirred selenium, be cooled to selenium
At 290 DEG C, then be stirred continuously 5 minutes, after above-mentioned selenium solution is cooled to 240~250 DEG C, pour into aluminium dish respectively, respectively from
The first, it is sampled in intermediate, last three disk, two parts is divided into after being mixed and finely ground, and analyze it brominated amount, brominated amount general control exists
1%, it is ground into diameter 10mm fritter below by selenium is added with mortar, is incorporated in the black port grinding bottle of lid, is stored in nice and cool
Dark cabinet in；
(7) the evaporation selenium described in: its operating process are as follows: it is pre- to open cooling water → station busbar connector → aluminium skin heating power supply
Hot 1.5h~2.5h → selenium stove heating power supply, opened Ventilating valve after 30 minutes, fell vacuum kettle, and selenium furnace temperature is 280~300
DEG C, aluminium skin heating power supply → operation charging switch is closed, selenium furnace is sailed to charging, selenium is fitted into furnace slot until 0.8cm,
The aluminium sheet of weighing is promoted into inserted slot bismuth downwards, loads onto aluminium sheet lid, selenium furnace is driven towards parking area, used by operation blowing out switch
Compressed air closes vacuum kettle, opens vacuum power；
(8) returning described in steams piece: its operating process are as follows: evaporation process is to open big pre- true after vacuum pump start-up operation
Empty pump valve, vacuumize 10~after twenty minutes, aluminium skin heating power supply is opened, is heated 3~4 minutes, heating power 1.5KW, to
Vacuum degree reaches 8Pa6 × 10-2When, manipulation evaporation switch connects furnace vehicle power supply, closes the heating of aluminium skin, start to evaporate, until rule
Determine evaporation time, after evaporation time is generally 12~15 minutes, furnace vehicle is sailed into parking area.Selenium layer 90~130g of weight demands,
Its weight error≤3% opens air inlet valve door, closes big fore pump, fall vacuum kettle, plugs safety pin, before taking out aluminium skin
End cap, presss from both sides out selenium piece with pliers, jaw intermediate plate 5mm weighs up the weight of selenium, piece vertically put into load vehicle, by weight
Filling record, continuous evaporation were opened the time≤4 minutes, and selenium piece of doing over again should evaporate in 4h after energizing in advance, and twice evaporation weight is
90~130g, interior is not allow for the mercury vapour of denier, with≤the 48h that energizes interval time in advance；
(9) pre- described in is energized: its operating process are as follows: power switch, motor switch are first turned on, by 6KW, 4KW, 2KW
It is fully open, the selenium piece of steamed selenium is inserted perpendicularly into vehicle of energizing, selenium face reply dress, per car puts loading amount≤30 piece after liner,
After furnace temperature reaches 110 DEG C, fire door is opened, completes track road of energizing, is pushed into vehicle of energizing, closes fire door, furnace temperature rises to 104 DEG C
It is to close 6KW, 4KW heater switch, when furnace temperature rises to 112 DEG C ± 2 DEG C because of inertia, controls 2KW or 4KW with contact thermometer, it is permanent
Warm 2h pulls out furnace vehicle after closing motor switch, power switch, after 10~15 minutes to be cooled, extracts selenium piece out and is packed into and deposit piece
Che Zhong, interior are not allow for the mercury vapour of denier；
(10) punching described in: its operating process are as follows: whether normal first check for each component of lathe, and soaked with clean cotton yarn
Alcohol wipe scissors and work top, press dark buttons, start shearing machine, and strip selenium piece is put into mold by predetermined size,
Punching is at qualification on punching machine152、222、302、402Selenium piece or in flakes, the connection piece that punching goes out, it is main energize after
It is put into certain mold, then punching is at qualified monolithic；
(11) the fusion gold described in: its operating process are as follows: 10 are weighed up by formula thallium g=(+32% cadmium of 68% tin) 2/0,000~
15kg produces tin, cadmium, thallium weight used in alloy process, dries aluminum alloy pan, the tin weighed up is put into pot, opens electricity and adds
Tin is heated to 350 DEG C by thermal switch, and when being cooled to 220~240 DEG C, the cadmium of title is added, opens vent cabinet, after to be dissolved,
It when temperature rises to 240 ± 10 DEG C, keeps this temperature to stir 30 minutes, goes out surface scum with bale-out, tin cadmium is added in the thallium weighed up
It in alloy, is kept for 240 ± 10 DEG C stir 30 minutes, goes out surface scum with bale-out, in aluminium alloy injection mould, close electric heating
Switch and vent cabinet；
(12) spray alloy and connection piece described in: its operating process are as follows: alloy bar is put into melting pot, electric furnace heating is opened and opens
It closes, after ternary alloy three-partalloy fusing, when temperature reaches 240 ± 10 DEG C, is controlled with thermocouple thermometer, operation opens spray gun before first 25 minutes
Heating power supply, appropriate adjustment heating power supply；Then dress cabinet is carried out, Selenium piece is upward, is placed on bottom plate, loads onto and covers
Lid button；60 × 60 selenium pieces are upward, are placed on bottom plate, and covering button is put into hole, and template and press box are filled, and tighten clip, will be closed with spoon
Gold injection spray gun, opens exhausting power supply and air compressor power supply；Spray alloy frame is entered into spray gun, air pressure is adjusted to 4 ± 0.2kg/cm2,
Lance head uniformly sprays alloy apart from selenium 8 ± 1.5cm of piece, takes out the selenium piece sprayed and carries out connection piece；
(13) master described in energizes: its operating process are as follows: 8KW stove is shifted to an earlier date 3 days and is preheated, is protected using contact thermometer
217 ± 5 DEG C of furnace temperature, transfer is opened, adjusts transformer, the control main time of energizing is between 26~40 minutes, in conveyer belt inlet
Selenium piece is put down, send naphthalene furnace to start master and energizes, remove selenium piece in exit, prediction is met the requirements, can be sent with reversed
Piece takes out to all commutator segments, closes transmission motor power；
(14) the selenium piece chamfering described in: its operating process are as follows: ready selenium piece is placed in location hole, is powered on out
It closes, push button switch, motor rotation corrects lathe tool depth according to the selenium piece of initial workpiece chamfering again, until qualified, selenium piece circle
Then the chamfer dimesion in week should take 5~10 friendships to examine and assert in 0.2 × 20 °~45 °, can give birth to after chamfer quality is qualified
It produces, good selenium piece heads into rewinding box by auto spring, after work, closes motor power, and selenium piece is delivered master and is energized；
(15) impact described in: its operating process are as follows: it is bright to power on switch C=100 μ f indicator light, by contact voltage pressure
It is bright to close short-circuit indicator light, selenium piece alloy is face-up, it is placed on contact electrode, adds 40V voltage, press contact electrode, if short-circuit
Indicator light does not work, and selenium piece is qualified, conversely, selenium piece short circuit, should increase capacitor stroke.If short circuit refers in C=500 μ f impact
Show that lamp is still bright, then plus 50V, 60V, 70V impact, the still bright person of short-circuit indicator light scrap, and by contact electrode pressing, short circuit makes capacitor
Device electric discharge, while voltage regulator/transformer is zeroed, disconnecting power switch；
(16) electrical reset and impact sieve described in: its operating process are as follows: plugged between instrument reverse side of energizing energizes electrode whole
Flow, alloy face same direction, check whether instrument each section switch of energizing is placed on correct position, adjust work according to room ambient conditions
Make, time of having a rest relay is normal, to guarantee requirement of energizing, opens platform total power switch of energizing, and connects start button switch, continuously
Operating switch adjusts voltage of energizing, and connects branch enabling key, connects branch tune short circuit current and switchs to short circuit, adjusting immediately can
Power transformation resistance, branch short switch is dialled in energising position, is removed selenium cell, after storage for 24 hours, then is carried out shock-testing operation,
Then the selenium cell of impact test passes is screened；
(17) reverse measuremenet described in: its operating process are as follows: put on rubber finger, take out selenium piece qualified after screening, root
Test desk is selected according to piece type, checks test desk instrument, regulated power supply switch can be connected after the check and correction quality certification is effective, test desk is opened
It closes, turns on the power switch, point-score commissioning amount voltage, selenium cell alloy is face-up, test pen are selected according to as defined in measurement table
It connects 5 seconds, whether sees current indication in acceptability limit, after measure, closing power supply and regulated power supply, the qualified product measured,
Turn to lead to measurement, rejected product continues electrical reset；
(18) lead to measurement: its operating process are as follows: test desk is selected according to piece type, puts on rubber finger, takes out selenium piece, inspection
After looking into measurement table qualification effectively, regulated power supply switch, test desk switch are connected, piece alloy is measured and faces upward, connects test test pencil,
Electric current is adjusted to rated value.It carries out leading to voltage measurement again after adjustment electric current, test desk switch is closed after measurement, regulated power supply is opened
It closes, selenium piece is placed in defined box by grouping requirement, is assembled or packed after passing the inspection；
(19) being packed at inspection described in, storage storage: after product inspection is qualified, according to packaging the piece number 152~402: every packet
200,602~1002: every packet 50 first wraps up one layer of moistureproof paper, then wrap up one layer of brown paper, selenium sheet gauge is beaten on brown paper
Lattice, model, red seal oil seal, the factory of selenium piece monolithic blue print classification, group, quantity, date seal, finally storage storage
It deposits.
The beneficial effects of the present invention are: due to using semiconductor selenium as main material, using special process process by selenium
Coated on commutator segment, selenium chip semiconductor element is formed, rectification and overload protection is enhanced, extends the semiconductor element service life,
Achieve the purpose that it is energy-saving, so that it is high to realize electric mass of system, light-weighted requirement.
Detailed description of the invention:
Fig. 1 is process flow chart of the invention.
Specific embodiment:
Embodiment 1: as shown in Figure 1, a kind of selenium cell of selenium cell preparation process be by being sliced, developing a film, sandblasting,
Drying, evaporation bismuth, selenium preparation, evaporation selenium, return steam piece, energize in advance, punching, fusion gold, spray alloy, connection piece, master energize, chamfering,
Impact, electrical reset, impact, sieve, reverse measuremenet, at inspection pack and storage storage process be prepared, concrete technology preparation
Process are as follows:
(1) slice described in: being that an aluminium sheet greatly is cut into 0.8mm × 1015mm × 2040mm size, tight during blank
Prohibit scratch surface, surface of aluminum plate has oxide layer that can not shear, and big aluminium sheet can not be sheared before shearing if any mechanical hard defects；
(2) developing a film described in: cleaning surface of aluminum plate greasy dirt with gasoline first, then cleans surface of aluminum plate oil again with buck
Dirt, the surface of aluminum plate cleaned answer light, without foul, aluminium sheet abraded area >=10mm2, should reject, not allow flow into lower road work
Sequence；
(3) sandblasting described in: its operating process are as follows: connection precipitator power supplies first pour into quartz sand in cabin, every shift
Add sand 60kg, 4 additions should be divided within full class's working time, about 15kg, must not once pour into, then check nozzle, connect every time
Again by stable gas pressure within the scope of 68.647~88.620KPa, i.e., logical sand-blasting machine linkage mechanism power supply opens compressed air valve
It can sandblasting；Aluminium sheet after sandblasting imports sandblasting wheel and removes again, finally identifies surface, should be light grey after aluminium sheet sandblasting, surface is not
Must there are serious black trace and luminous point, need 39.227~88.260KPa air pressure to respray once if any light；
(4) drying described in: its operating process are as follows: aluminium sheet is loaded vertically into drying vehicle, master switch is opened and opens air blast
Machine is connected heating 12KW and is all switched.Drying vehicle equipped with aluminium sheet is promoted in furnace, stove first preheats before working, fire door is shut,
Furnace temperature is heated to 175 ± 5 DEG C in 15 minutes, keeps the temperature 2h, after reaching temperature, is suitably heated with 4KW or 2KW, constant temperature is carried out, is dried
After dry, heater switch is disconnected, closes air blower, disconnects master switch, pulls out load vehicle；The aluminium sheet natural cooling 10 dried~
15 minutes, be put into load vehicle, with evaporation bismuth interval time≤4h, should put in baker and save more than 4h, deposit the piece time be more than for 24 hours,
It should be dried 30 minutes again with 100~120 DEG C；
(5) the evaporation bismuth described in: its operating process are as follows: open bismuth pot gas valve, fall vacuum kettle, and plug safety
Pin, the frame for installing aluminium sheet≤20, is deposited in storage shelf, in addition cover board, hangs up support welding block, the small bismuth pot number of pressing is put into
In furnace, every pot of bismuth weight 45g ± 1g；
Evaporating bismuth process is to close big fore pump air inlet valve door, opens big fore pump, and opening is pre- greatly to pump logical pot valve,
It when vacuum degree reaches 2.666Pa, opens diffusion pump and leads to pot valve, close big pre- pump vacuum valve, the moment is in parallel with diffusion pump, beats
It opens and is pumped into air valve in advance greatly, close big pre- pump and cooling water, adjust aluminium sheet counter；When vacuum degree reaches 0.666Pa, bismuth is connected
Pot heater switch, heating are evaporated automatically after 15 minutes, and evaporation time is adjusted to 2~4 minutes, and according to upper one pot of bismuth layer, adjust bismuth
Pot power, record steam first, intermediate a piece of, last a piece of vacuum degree, have steamed last a piece of alarm whistle, closed report sound
Device switch, diffusion pump valve and heating power supply, three ten minutes later, opens Ventilating valve, falls vacuum kettle, disengages rotation clutch
Device removes baffle block, takes out the bismuth piece evaporated and is put into load vehicle, send selenium to evaporate after the assay was approved；Bismuth piece is stored in product
≤ 6h, interior, which does not allow to store, to be had and micro mercury vapour and various oils and volatile article, can not be caused on aluminium sheet
Scuffing, mechanical damage, greasy dirt, impression of the hand can not make aluminium sheet deformation；
(6) the selenium preparation described in: its operating process are as follows: weigh out the selenium powder of two parts of 70g in the balance, portion is poured on ground triangle
In beaker, 15ml liquid bromine is measured with graduated cylinder, is poured in conical flask, speed should slowly and constantly shake, will be another in beaker
Part 70ml selenium powder shake is slowly poured into triangular flask, is then closed the lid, and after storing 48h, can configure addition selenium；
System addition selenium, weighs up 5kg selenium, is poured into stainless steel agitated kettle, and heating fusing is stirred at 300~350 DEG C
2h is clamped equipped with selenium bromide triangular flask bottleneck with clamp, after dissolving on electric furnace, is poured into stirred selenium, be cooled to selenium
At 290 DEG C, then be stirred continuously 5 minutes, after above-mentioned selenium solution is cooled to 240~250 DEG C, pour into aluminium dish respectively, respectively from
The first, it is sampled in intermediate, last three disk, two parts is divided into after being mixed and finely ground, and analyze it brominated amount, brominated amount general control exists
1%, it is ground into diameter 10mm fritter below by selenium is added with mortar, is incorporated in the black port grinding bottle of lid, is stored in nice and cool
Dark cabinet in；
(7) the evaporation selenium described in: its operating process are as follows: it is pre- to open cooling water → station busbar connector → aluminium skin heating power supply
Hot 1.5h~2.5h → selenium stove heating power supply, opened Ventilating valve after 30 minutes, fell vacuum kettle, and selenium furnace temperature is 280~300
DEG C, aluminium skin heating power supply → operation charging switch is closed, selenium furnace is sailed to charging, selenium is fitted into furnace slot until 0.8cm,
The aluminium sheet of weighing is promoted into inserted slot bismuth downwards, loads onto aluminium sheet lid, selenium furnace is driven towards parking area, used by operation blowing out switch
Compressed air closes vacuum kettle, opens vacuum power；
(8) returning described in steams piece: its operating process are as follows: evaporation process is to open big pre- true after vacuum pump start-up operation
Empty pump valve, vacuumize 10~after twenty minutes, aluminium skin heating power supply is opened, is heated 3~4 minutes, heating power 1.5KW, to
Vacuum degree reaches 8Pa6 × 10-2When, manipulation evaporation switch connects furnace vehicle power supply, closes the heating of aluminium skin, start to evaporate, until rule
Determine evaporation time, after evaporation time is generally 12~15 minutes, furnace vehicle is sailed into parking area.Selenium layer 90~130g of weight demands,
Its weight error≤3% opens air inlet valve door, closes big fore pump, fall vacuum kettle, plugs safety pin, before taking out aluminium skin
End cap, presss from both sides out selenium piece with pliers, jaw intermediate plate 5mm weighs up the weight of selenium, piece vertically put into load vehicle, by weight
Filling record, continuous evaporation were opened the time≤4 minutes, and selenium piece of doing over again should evaporate in 4h after energizing in advance, and twice evaporation weight is
90~130g, interior is not allow for the mercury vapour of denier, with≤the 48h that energizes interval time in advance；
(9) pre- described in is energized: its operating process are as follows: power switch, motor switch are first turned on, by 6KW, 4KW, 2KW
It is fully open, the selenium piece of steamed selenium is inserted perpendicularly into vehicle of energizing, selenium face reply dress, per car puts loading amount≤30 piece after liner,
After furnace temperature reaches 110 DEG C, fire door is opened, completes track road of energizing, is pushed into vehicle of energizing, closes fire door, furnace temperature rises to 104 DEG C
It is to close 6KW, 4KW heater switch, when furnace temperature rises to 112 DEG C ± 2 DEG C because of inertia, controls 2KW or 4KW with contact thermometer, it is permanent
Warm 2h pulls out furnace vehicle after closing motor switch, power switch, after 10~15 minutes to be cooled, extracts selenium piece out and is packed into and deposit piece
Che Zhong, interior are not allow for the mercury vapour of denier；
(10) punching described in: its operating process are as follows: whether normal first check for each component of lathe, and soaked with clean cotton yarn
Alcohol wipe scissors and work top, press dark buttons, start shearing machine, and strip selenium piece is put into mold by predetermined size,
Punching is at qualification on punching machine152、222、302、402Selenium piece or in flakes, the connection piece that punching goes out, it is main energize after
It is put into certain mold, then punching is at qualified monolithic；
(11) the fusion gold described in: its operating process are as follows: 10 are weighed up by formula thallium g=(+32% cadmium of 68% tin) 2/0,000~
15kg produces tin, cadmium, thallium weight used in alloy process, dries aluminum alloy pan, the tin weighed up is put into pot, opens electricity and adds
Tin is heated to 350 DEG C by thermal switch, and when being cooled to 220~240 DEG C, the cadmium of title is added, opens vent cabinet, after to be dissolved,
It when temperature rises to 240 ± 10 DEG C, keeps this temperature to stir 30 minutes, goes out surface scum with bale-out, tin cadmium is added in the thallium weighed up
It in alloy, is kept for 240 ± 10 DEG C stir 30 minutes, goes out surface scum with bale-out, in aluminium alloy injection mould, close electric heating
Switch and vent cabinet；
(12) spray alloy and connection piece described in: its operating process are as follows: alloy bar is put into melting pot, electric furnace heating is opened and opens
It closes, after ternary alloy three-partalloy fusing, when temperature reaches 240 ± 10 DEG C, is controlled with thermocouple thermometer, operation opens spray gun before first 25 minutes
Heating power supply, appropriate adjustment heating power supply；Then dress cabinet is carried out, Selenium piece is upward, is placed on bottom plate, loads onto and covers
Lid button；60 × 60 selenium pieces are upward, are placed on bottom plate, and covering button is put into hole, and template and press box are filled, and tighten clip, will be closed with spoon
Gold injection spray gun, opens exhausting power supply and air compressor power supply；Spray alloy frame is entered into spray gun, air pressure is adjusted to 4 ± 0.2kg/cm2,
Lance head uniformly sprays alloy apart from selenium 8 ± 0.5cm of piece, takes out the selenium piece sprayed and carries out connection piece；
(13) master described in energizes: its operating process are as follows: 8KW stove is shifted to an earlier date 3 days and is preheated, is protected using contact thermometer
217 ± 5 DEG C of furnace temperature, transfer is opened, adjusts transformer, the control main time of energizing is between 26~40 minutes, in conveyer belt inlet
Selenium piece is put down, send naphthalene furnace to start master and energizes, remove selenium piece in exit, prediction is met the requirements, can be sent with reversed
Piece takes out to all commutator segments, closes transmission motor power；
(14) the selenium piece chamfering described in: its operating process are as follows: ready selenium piece is placed in location hole, is powered on out
It closes, push button switch, motor rotation corrects lathe tool depth according to the selenium piece of initial workpiece chamfering again, until qualified, selenium piece circle
Then the chamfer dimesion in week should take 5~10 friendships to examine and assert in 0.2 × 20 °~45 °, can give birth to after chamfer quality is qualified
It produces, good selenium piece heads into rewinding box by auto spring, after work, closes motor power, and selenium piece is delivered master and is energized；
(15) impact described in: its operating process are as follows: it is bright to power on switch C=100 μ f indicator light, by contact voltage pressure
It is bright to close short-circuit indicator light, selenium piece alloy is face-up, it is placed on contact electrode, adds 40V voltage, press contact electrode, if short-circuit
Indicator light does not work, and selenium piece is qualified, conversely, selenium piece short circuit, should increase capacitor stroke.If short circuit refers in C=500 μ f impact
Show that lamp is still bright, then plus 50V, 60V, 70V impact, the still bright person of short-circuit indicator light scrap, and by contact electrode pressing, short circuit makes capacitor
Device electric discharge, while voltage regulator/transformer is zeroed, disconnecting power switch；
(16) electrical reset and impact sieve described in: its operating process are as follows: plugged between instrument reverse side of energizing energizes electrode whole
Flow, alloy face same direction, check whether instrument each section switch of energizing is placed on correct position, adjust work according to room ambient conditions
Make, time of having a rest relay is normal, to guarantee requirement of energizing, opens platform total power switch of energizing, and connects start button switch, continuously
Operating switch adjusts voltage of energizing, and connects branch enabling key, connects branch tune short circuit current and switchs to short circuit, adjusting immediately can
Power transformation resistance, branch short switch is dialled in energising position, is removed selenium cell, after storage for 24 hours, then is carried out shock-testing operation,
Then the selenium cell of impact test passes is screened；
(17) reverse measuremenet described in: its operating process are as follows: put on rubber finger, take out selenium piece qualified after screening, root
Test desk is selected according to piece type, checks test desk instrument, regulated power supply switch can be connected after the check and correction quality certification is effective, test desk is opened
It closes, turns on the power switch, point-score commissioning amount voltage, selenium cell alloy is face-up, test pen are selected according to as defined in measurement table
It connects 5 seconds, whether sees current indication in acceptability limit, after measure, closing power supply and regulated power supply, the qualified product measured,
Turn to lead to measurement, rejected product continues electrical reset；
(18) lead to measurement: its operating process are as follows: test desk is selected according to piece type, puts on rubber finger, takes out selenium piece, inspection
After looking into measurement table qualification effectively, regulated power supply switch, test desk switch are connected, piece alloy is measured and faces upward, connects test test pencil,
Electric current is adjusted to rated value.It carries out leading to voltage measurement again after adjustment electric current, test desk switch is closed after measurement, regulated power supply is opened
It closes, selenium piece is placed in defined box by grouping requirement, is assembled or packed after passing the inspection；
(19) being packed at inspection described in, storage storage: after product inspection is qualified, according to packaging the piece number 152~402: every packet
200,602~1002: every packet 50 first wraps up one layer of moistureproof paper, then wrap up one layer of brown paper, selenium sheet gauge is beaten on brown paper
Lattice, model, red seal oil seal, the factory of selenium piece monolithic blue print classification, group, quantity, date seal, finally storage storage
It deposits.
Embodiment 2: as shown in Figure 1, (6) the selenium preparation production selenium process of selenium cell preparation process a kind of are as follows: claim
Selenium to be prepared is needed out, is poured into stainless steel selenium pot, and it is 2~8h that heating, which is melted to 300~350 DEG C of mixings time, is cooled to
At 290 DEG C, the dross on selenium surface being removed, the addition selenium weighed up is then added, keeps stirring, 10~40kg need to stir 10~
20 minutes, addition selenium quantity was calculated by actual production selenium weight in pot, after being cooled to 240~250 DEG C, was poured into aluminium dish respectively,
The selenium poured out should be black, when should avoid temperature is low from not coming out rapidly, the selenium that will be prepared, respectively from first, it is intermediate,
It being sampled in last three disk, two parts is divided into after being mixed and finely ground, and analyze it brominated amount, remaining mounted box, number are simultaneously placed on selenium frame,
The generally brominated amount of this selenium is not to be exceeded ± the 20% of specified amount, and selenium evaporation is received by qualified notification sheet.
Embodiment 3: as shown in Figure 1, the 4. of a kind of selenium cell preparation process according to claim 1 described one
Kind selenium arranges piece preparation process, it is characterized in that: according to the brominated amount analysis of addition selenium as a result, meter in described (6) the selenium preparation process
Calculate the addition weight that should be added in production selenium；
Calculate publicity a=B × A/C
Selenium weight is added needed for a---
Production Se content is made needed for B---
A--- is packed into the selenium powder weight in agitated kettle
C--- adds the average brominated amount in selenium.
As shown in Figure 1, in (6) selenium preparation process of selenium cell preparation process a kind of in selenium bromine measurement: respectively
The analysis sample for taking production 2~5g of selenium, adding 1~2g of selenium, is put into glass mortar and is ground into powder.It is ground with ox horn bale-out
Good selenium powder is placed on 1~5g of weighing on precision balance；Load weighted selenium powder, the capacity 500ml triangle after pouring into cleaning and drying
In flask；
Will preparatory measured silver nitrate solution 0.01N, instilled in conical flask with sour dropper, it is general produce selenium drop 12~
15ml, addition selenium drip 20~25ml；50ml silver nitrate is weighed with graduated cylinder, is poured into triangular flask；Filling sample silver nitrate, nitric acid
Conical flask, be put into water-bath, low-temperature heat, about 100 DEG C of water bath temperature；
In selenium course of dissolution, a large amount of nitrogen dioxide gas will be generated, is volatilized completely to nitrogen dioxide gas, selenium whole
After dissolution, triangular flask is removed immediately, outer wall is rinsed with tap water, is substantially cooled to room temperature, absolute prohibition water droplet enters in bottle；
It measures 5ml toluene to pour into triangular flask, measures 5ml saturation ferriammonium sulfate solution and pour into triangular flask；Sulphation is measured with sour dropper
Ammonium salt solution 0.01N is titrated, and in titration process, excessive silver nitrate solution in conical flask is initially transparent, slightly pale green
Color is afterwards milky white liquid, until rocking when some pale reds are presented uniformly, finally by the rhodan ammonium data of titration
Ml is recorded.
Embodiment 4: as shown in Figure 1, a kind of selenium cell preparation process's prepares solution in (6) selenium preparation process
And calibration are as follows:
Weigh with scale the rhodan ammonium of 0.7612gAR in preparation, is put into the narrow-mouthed bottle of 1000ml, adds distilled water, dilute
It releases to 1000ml, shakes uniformly；
0.0400g metallic silver (accuracy 0.0001g) is weighed with precision balance in calibration, the triangle for being put into 300ml is burnt
In bottle, 10ml1: 1 HNO is added3It first shakes, makes silver-colored dissolution, then heating makes silver-colored all dissolutions on electric furnace, and when heating infuses
Meaning overflows solution, and after nitrogen dioxide gas is evaporated completely, and stops heating, is cooled down, simultaneously with distilled water flushing bottle wall
About 100ml is diluted, after shaking uniformly, saturation ferriammonium sulfate solution is added, is titrated immediately with prepared rhodan ammonium, shaken in drop
It is even, until being in brick-red.
Calculation formula: NH4CN5Concentration-N
N=Ag (1g)/NH4CN5(ml)0.10788
The preparation process of its ferriammonium sulfate solution are as follows:
Container to be cleaned drying, is weighed according to ammonium ferric sulfate solubility, 100g water is 44.15g at 25 DEG C of room temperature,
About 500g every time, is then put into the solid sulphuric acid iron ammonium weighed up in distilled water, is filbert after dissolution, then with 1: 1 nitric acid
Titration, brown disappear, and in until yellow green, solution can be used by filtering rear；
The preparation and calibration of its silver nitrate solution are as follows:
Weigh with scale the silver nitrate of 1.6989gAR in preparation, is put into the narrow-mouthed bottle of 1000ml, adds a small amount of distillation
Water after dissolution, dilutes 1000ml with distilled water, shakes uniformly；
The silver nitrate solution 20ml or so newly prepared in calibration with dropper, is poured into the triangular flask of 300ml, dilute with distilled water
About 100ml is released, 1ml is added and is saturated ferriammonium sulfate solution, with the rhodan ammonium solution of known concentration, is shaken in drop, until dripping to out
Until existing red, take reading；
Calculation formula: AgNO3Concentration N
N=NH4CNS(ML)×NH4CNS (concentration)/taking-up AgNO3Volume ml.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of selenium cell preparation process, it is characterized in that: selenium cell be by being sliced, developing a film, sandblasting, drying, evaporation bismuth,
Selenium preparation, evaporation selenium, return steam piece, energize in advance, punching, fusion gold, spray alloy, connection piece, master energize, chamfering, impact, electrical reset,
Impact, sieve, reverse measuremenet, at inspection pack and storage storage process be prepared, concrete technology preparation process are as follows:
(1) slice described in: it is that an aluminium sheet greatly is cut into 0.8mm × 1015mm × 2040mm size, forbids to draw during blank
Hurt surface, surface of aluminum plate has oxide layer that can not shear, and big aluminium sheet can not be sheared before shearing if any mechanical hard defects；
(2) developing a film described in: cleaning surface of aluminum plate greasy dirt with gasoline first, then clean surface of aluminum plate greasy dirt again with buck, wipes
Washed surface of aluminum plate answers light, without foul, aluminium sheet abraded area >=10mm2, should reject, not allow flow into next procedure；
(3) sandblasting described in: its operating process are as follows: connection precipitator power supplies first pour into quartz sand in cabin, every shift adds sand
60kg should divide 4 additions within full class's working time, and about 15kg, must not once pour into every time, then check nozzle, connect spray
Sand machine linkage mechanism power supply is opened compressed air valve again by stable gas pressure within the scope of 68.647~88.620KPa, can be sprayed
Sand；Aluminium sheet after sandblasting imports sandblasting wheel and removes again, finally identifies surface, should be light grey after aluminium sheet sandblasting, surface must not have
Serious black trace and luminous point need 39.227~88.260KPa air pressure to respray once if any light；
(4) drying described in: its operating process are as follows: aluminium sheet is loaded vertically into drying vehicle, master switch is opened and opens air blower, connect
Logical heating 12KW is all switched.It will be promoted in furnace equipped with the drying vehicle of aluminium sheet, stove first preheats before working, shut fire door, 15 points
Furnace temperature is heated to 175 ± 5 DEG C in clock, keeps the temperature 2h, after reaching temperature, is suitably heated with 4KW or 2KW, constant temperature is carried out, has dried
Bi Hou disconnects heater switch, closes air blower, disconnects master switch, pulls out load vehicle；10~15 points of the aluminium sheet natural cooling dried
Clock is put into load vehicle, with evaporation bismuth interval time≤4h, should put in baker and save more than 4h, deposit the piece time be more than for 24 hours, should be with
100~120 DEG C dry 30 minutes again；
(5) the evaporation bismuth described in: its operating process are as follows: bismuth pot gas valve is opened, falls vacuum kettle, and plug safety pin,
The frame for installing aluminium sheet≤20, is deposited in storage shelf, in addition cover board, hangs up support welding block, the small bismuth pot number of pressing is put into furnace,
Every pot of bismuth weight 45g ± 1g；
Evaporating bismuth process is to close big fore pump air inlet valve door, opens big fore pump, and opening is pre- greatly to pump logical pot valve, vacuum
It when degree reaches 2.666Pa, opens diffusion pump and leads to pot valve, close big pre- pump vacuum valve, the moment is in parallel with diffusion pump, opens big
It is pumped into air valve in advance, closes big pre- pump and cooling water, adjusts aluminium sheet counter；When vacuum degree reaches 0.666Pa, connects bismuth pot and add
Thermal switch, heating are evaporated automatically after 15 minutes, and evaporation time is adjusted to 2~4 minutes, and according to upper one pot of bismuth layer, adjust bismuth pot function
Rate, record steam first, intermediate a piece of, last a piece of vacuum degree, have steamed last a piece of alarm whistle, closed alarm and open
It closes, spread pump valve and heating power supply, three ten minutes later, opens Ventilating valve, falls vacuum kettle, disengages rotation clutch, takes
Lower block tile is taken out the bismuth piece evaporated and is put into load vehicle, send selenium to evaporate after the assay was approved；Bismuth piece in product storage≤6h,
Interior, which does not allow to store, to be had and micro mercury vapour and various oils and volatile article, can not cause to scratch on aluminium sheet,
Mechanical damage, greasy dirt, impression of the hand can not make aluminium sheet deformation；
(6) the selenium preparation described in: its operating process are as follows: weigh out the selenium powder of two parts of 70g in the balance, portion is poured on ground conical beaker
In, 15ml liquid bromine is measured with graduated cylinder, is poured in conical flask, speed should slowly and constantly shake, by another in beaker
The shake of 70ml selenium powder is slowly poured into triangular flask, is then closed the lid, and after storing 48h, can configure addition selenium；
System addition selenium, weighs up 5kg selenium, is poured into stainless steel agitated kettle, and heating fusing stirs 2h at 300~350 DEG C,
It is clamped with clamp equipped with selenium bromide triangular flask bottleneck, after being dissolved on electric furnace, pours into stirred selenium, be cooled to 290 to selenium
DEG C when, then be stirred continuously 5 minutes, after above-mentioned selenium solution is cooled to 240~250 DEG C, pour into aluminium dish respectively, respectively from
One, it is sampled in intermediate, last three disk, two parts is divided into after being mixed and finely ground, and analyze it brominated amount, brominated amount general control exists
1%, it is ground into diameter 10mm fritter below by selenium is added with mortar, is incorporated in the black port grinding bottle of lid, is stored in nice and cool
Dark cabinet in；
(7) the evaporation selenium described in: its operating process are as follows: open cooling water → station busbar connector → aluminium skin heating power supply preheating
1.5h~2.5h → selenium stove heating power supply, opened Ventilating valve after 30 minutes, fell vacuum kettle, and selenium furnace temperature is 280~300
DEG C, aluminium skin heating power supply → operation charging switch is closed, selenium furnace is sailed to charging, selenium is fitted into furnace slot until 0.8cm,
The aluminium sheet of weighing is promoted into inserted slot bismuth downwards, loads onto aluminium sheet lid, selenium furnace is driven towards parking area, used by operation blowing out switch
Compressed air closes vacuum kettle, opens vacuum power；
(8) returning described in steams piece: its operating process are as follows: evaporation process is to open big fore pump after vacuum pump start-up operation
Valve, vacuumize 10~after twenty minutes, aluminium skin heating power supply is opened, is heated 3~4 minutes, heating power 1.5KW, to vacuum
Degree reaches 8Pa6 × 10-2When, manipulation evaporation switch connects furnace vehicle power supply, closes the heating of aluminium skin, start to evaporate, until regulation is steamed
The time is sent out, after evaporation time is generally 12~15 minutes, furnace vehicle is sailed into parking area.Selenium layer weight demands 90~130g is heavy
Error≤3% is measured, air inlet valve door is opened, closes big fore pump, fall vacuum kettle, plugs safety pin, takes out aluminium skin drive end bearing bracket
Son presss from both sides out selenium piece with pliers, and jaw intermediate plate 5mm weighs up the weight of selenium, piece is vertically put into load vehicle, weight is inserted
Record, continuous evaporation opened the time≤4 minutes, and selenium piece of doing over again should evaporate in 4h after energizing in advance, and twice evaporation weight is 90~
130g, interior is not allow for the mercury vapour of denier, with≤the 48h that energizes interval time in advance；
(9) pre- described in is energized: its operating process are as follows: power switch, motor switch is first turned on, by 6KW, 4KW, 2KW whole
It opens, the selenium piece of steamed selenium is inserted perpendicularly into vehicle of energizing, selenium face reply dress, per car puts loading amount≤30 piece after liner, in furnace temperature
After reaching 110 DEG C, fire door is opened, completes track road of energizing, is pushed into vehicle of energizing, closes fire door, furnace temperature, which rises to 104 DEG C, is, closes
6KW, 4KW heater switch are closed, when furnace temperature rises to 112 DEG C ± 2 DEG C because of inertia, controls 2KW or 4KW, constant temperature 2h with contact thermometer,
After closing motor switch, power switch, furnace vehicle is pulled out, after 10~15 minutes to be cooled, selenium piece is extracted out and is fitted into and deposit in piece vehicle,
Interior is not allow for the mercury vapour of denier；
(10) punching described in: its operating process are as follows: it is whether normal and smart with clean cotton yarn infusing drugs in wine to first check for each component of lathe
Scissors and work top are wiped, dark buttons is pressed, starts shearing machine, strip selenium piece is put into mold by predetermined size, is being rushed
Punching is at qualified ￠ 5, ￠ 7,15 on bed2、222、302、402Selenium piece or in flakes, the connection piece that punching goes out, it is main energize after be put into one
In fixed mold, then punching is at qualified monolithic；
(11) the fusion gold described in: its operating process are as follows: weigh up 10~15kg by formula thallium g=(+32% cadmium of 68% tin) 2/0,000
Tin, cadmium, thallium weight used in alloy process are produced, aluminum alloy pan is dried, the tin weighed up is put into pot, electric heating is opened and opens
It closes, tin is heated to 350 DEG C, when being cooled to 220~240 DEG C, the cadmium of title is added, opens vent cabinet, after to be dissolved, temperature
It when rising to 240 ± 10 DEG C, keeps this temperature to stir 30 minutes, goes out surface scum with bale-out, tin cadmium alloy is added in the thallium weighed up
In, it is kept for 240 ± 10 DEG C stir 30 minutes, goes out surface scum with bale-out, in aluminium alloy injection mould, close electric heating switch
And vent cabinet；
(12) spray alloy and connection piece described in: its operating process are as follows: alloy bar is put into melting pot, opens electric furnace heater switch,
It after ternary alloy three-partalloy fusing, when temperature reaches 240 ± 10 DEG C, is controlled with thermocouple thermometer, operation is opened spray gun before first 25 minutes and added
Thermoelectric generator, appropriate adjustment heating power supply；Then dress cabinet is carried out, the selenium piece of ￠ 5-40 × 40 is upward, is placed on bottom plate, loads onto covering
Button；60 × 60 selenium pieces are upward, are placed on bottom plate, and covering button is put into hole, and template and press box are filled, and tighten clip, with spoon by alloy
Spray gun is injected, exhausting power supply and air compressor power supply are opened；Spray alloy frame is entered into spray gun, air pressure is adjusted to 4 ± 0.2kg/cm2,Spray
Pipette tips uniformly spray alloy apart from selenium 8 ± 0.5cm of piece, take out the selenium piece sprayed and carry out connection piece；
(13) master described in energizes: its operating process are as follows: 8KW stove is shifted to an earlier date 3 days and is preheated, protects furnace temperature using contact thermometer
217 ± 5 DEG C, transfer is opened, adjusts transformer, the control main time of energizing is to face between 26~40 minutes in conveyer belt inlet
Under put selenium piece, send naphthalene furnace to start master and energize, remove selenium piece in exit, prediction is met the requirements, can send piece with reversed, to
All commutator segments take out, and close transmission motor power；
(14) the selenium piece chamfering described in: its operating process are as follows: ready selenium piece is placed in location hole, switch is powered on,
Push button switch, motor rotation correct lathe tool depth according to the selenium piece of initial workpiece chamfering again, until it is qualified, selenium piece circumference
Then chamfer dimesion should take 5~10 friendships to examine and assert in 0.2 × 20 °~45 °, can produce after chamfer quality is qualified,
Good selenium piece heads into rewinding box by auto spring, after work, closes motor power, and selenium piece is delivered master and is energized；
(15) impact described in: its operating process are as follows: it is bright to power on switch C=100 μ f indicator light, contact voltage is pressed short
Road indicator light is bright, and selenium piece alloy is face-up, is placed on contact electrode, adds 40V voltage, press contact electrode, if short circuit instruction
Lamp does not work, and selenium piece is qualified, conversely, selenium piece short circuit, should increase capacitor stroke.If in C=500 μ f impact, short-circuit indicator light
Still bright, then plus 50V, 60V, 70V impact, the still bright person of short-circuit indicator light scrap, and by contact electrode pressing, short circuit puts capacitor
Electricity, while voltage regulator/transformer is zeroed, disconnecting power switch；
(16) electrical reset and impact sieve described in: its operating process are as follows: commutator segment is plugged between instrument reverse side of energizing energizes electrode,
Alloy faces same direction, checks whether instrument each section switch of energizing is placed on correct position, adjusts work according to room ambient conditions, not
It is normal to cease the time relay, to guarantee requirement of energizing, opens platform total power switch of energizing, connects start button switch, continuous work
Switch adjusts voltage of energizing, and connects branch enabling key, connects branch tune short circuit current and switchs to short circuit, adjusting immediately can power transformation
Resistance dials branch short switch in energising position, removes selenium cell, after storage for 24 hours, then carries out shock-testing operation, then
The selenium cell of impact test passes is screened；
(17) reverse measuremenet described in: its operating process are as follows: put on rubber finger, selenium piece qualified after screening is taken out, according to piece
Type selects test desk, checks test desk instrument, and regulated power supply switch, test desk switch can be connected after the check and correction quality certification is effective,
It turns on the power switch, point-score commissioning amount voltage is selected according to as defined in measurement table, selenium cell alloy is face-up, and test pen is connected
5 seconds, whether current indication was seen in acceptability limit, after having measured, closes power supply and regulated power supply, the qualified product measured turns logical
To measurement, rejected product continues electrical reset；
(18) lead to measurement: its operating process are as follows: test desk is selected according to piece type, puts on rubber finger, takes out selenium piece, checks and surveys
After scale qualification is effective, regulated power supply switch, test desk switch are connected, piece alloy is measured and faces upward, connection test test pencil will be electric
Stream is adjusted to rated value.It carries out leading to voltage measurement again after adjustment electric current, test desk switch, regulated power supply switch is closed after measurement,
Selenium piece is placed in defined box by grouping requirement, is assembled or packed after passing the inspection；
(19) being packed at inspection described in, storage storage: after product inspection is qualified, according to packaging the piece number 152~402: every packet 200
Piece, 602~1002: every packet 50 first wraps up one layer of moistureproof paper, then wraps up one layer of brown paper, beaten on brown paper selenium piece specification,
Model, red seal oil seal, the factory of selenium piece monolithic blue print classification, group, quantity, date seal, finally storage storage.
2. a kind of selenium cell preparation process according to claim 1, it is characterized in that: (6) the selenium preparation production selenium
Process are as follows: weighing up needs selenium to be prepared, pours into stainless steel selenium pot, heating be melted to 300~350 DEG C of mixings time be 2~
8h when being cooled to 290 DEG C, the dross on selenium surface is removed, the addition selenium weighed up is then added, keeps stirring, 10~
40kg need to be stirred 10~20 minutes, and addition selenium quantity is calculated by actual production selenium weight in pot, after being cooled to 240~250 DEG C, point
Do not pour into aluminium dish, the selenium poured out should be black, when should rapidly, avoid the low selenium that does not come out, will prepare of temperature, respectively
It is sampled from first, centre, last three disk, two parts is divided into after being mixed and finely ground, and analyze it brominated amount, remaining mounted box, number
And place on selenium frame, the generally brominated amount of this selenium is not to be exceeded ± the 20% of specified amount, and selenium evaporation is received by qualified notification sheet.
3. a kind of selenium cell preparation process according to claim 1, it is characterized in that: in described (6) the selenium preparation process
According to the brominated amount analysis of addition selenium as a result, calculating the addition weight that should be added in production selenium；
Calculate publicity a=B × A/C
Selenium weight is added needed for a---
Production Se content is made needed for B---
A--- is packed into the selenium powder weight in agitated kettle
C--- adds the average brominated amount in selenium.
4. a kind of selenium cell preparation process according to claim 1, it is characterized in that: in described (6) the selenium preparation process
The measurement of bromine in selenium: the analysis sample for taking production 2~5g of selenium respectively, adding 1~2g of selenium is put into grind into powder in glass mortar
Shape.With the selenium powder that ox horn bale-out is ground, it is placed on 1~5g of weighing on precision balance；Load weighted selenium powder pours into cleaning and drying
In capacity 500ml conical flask afterwards；
Preparatory measured silver nitrate solution 0.01N is generally produced selenium and is dripped 12~15ml in sour dropper instillation conical flask,
It adds selenium and drips 20~25ml；50ml silver nitrate is weighed with graduated cylinder, is poured into triangular flask；Filling the three of sample silver nitrate, nitric acid
Angle flask, is put into water-bath, low-temperature heat, and about 100 DEG C of water bath temperature；
In selenium course of dissolution, a large amount of nitrogen dioxide gas will be generated, is volatilized completely to nitrogen dioxide gas, selenium all dissolves
Afterwards, triangular flask is removed immediately, rinses outer wall with tap water, is substantially cooled to room temperature, absolute prohibition water droplet enters in bottle；It measures
5ml toluene pours into triangular flask, measures 5ml saturation ferriammonium sulfate solution and pours into triangular flask；It is molten that sulphation ammonium is measured with sour dropper
Liquid 0.01N is titrated, and in titration process, excessive silver nitrate solution in conical flask is initially transparent, slightly light green,
It is afterwards milky white liquid, until rocking uniformly when some pale reds are presented, finally remembering the rhodan ammonium data ml of titration
Record is got off.
5. a kind of selenium cell preparation process according to claim 4, it is characterized in that: described in (6) selenium preparation process
In prepare solution and calibration are as follows:
Weigh with scale the rhodan ammonium of 0.7612gAR in preparation, is put into the narrow-mouthed bottle of 1000ml, adds distilled water, is diluted to
1000ml shakes uniformly；
0.0400g metallic silver (accuracy 0.0001g) is weighed with precision balance in calibration, is put into the conical flask of 300ml,
Add 10ml1: 1 HNO3It first shakes, makes silver-colored dissolution, then heating makes silver-colored all dissolutions on electric furnace, and when heating pays attention to not making
Solution overflows, and after nitrogen dioxide gas is evaporated completely, and stops heating, is cooled down, and with distilled water flushing bottle wall and dilutes about
100ml after shaking uniformly, adds saturation ferriammonium sulfate solution, is titrated immediately with prepared rhodan ammonium, shakes up in drop, directly
Until being in brick-red.
Calculation formula: NH4CN5Concentration-N
N=Ag (1g)/NH4CN5(ml)0.10788
The preparation process of its ferriammonium sulfate solution are as follows:
Container is cleaned drying, is weighed according to ammonium ferric sulfate solubility, 100g water is 44.15g at 25 DEG C of room temperature, every time about
For 500g, then the solid sulphuric acid iron ammonium weighed up is put into distilled water, is filbert after dissolution, then titrated with 1: 1 nitric acid, it is brown
Decoloration, in until yellow green, solution can be used by filtering rear；
The preparation and calibration of its silver nitrate solution are as follows:
Weigh with scale the silver nitrate of 1.6989gAR in preparation, is put into the narrow-mouthed bottle of 1000ml, adds a small amount of distilled water, molten
Xie Hou dilutes 1000ml with distilled water, shakes uniformly；
The silver nitrate solution 20ml or so newly prepared in calibration with dropper, is poured into the triangular flask of 300ml, about with distilled water dilution
100ml is added 1ml and is saturated ferriammonium sulfate solution, with the rhodan ammonium solution of known concentration, shakes in drop, until it is red to drip to appearance
Until color, take reading；
Calculation formula: AgNO3Concentration N
N=NH4CNS(ML)×NH4CNS (concentration)/taking-up AgNO3Volume ml.
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