CN109273355B - Preparation process of selenium rectifying sheet - Google Patents

Preparation process of selenium rectifying sheet Download PDF

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Publication number
CN109273355B
CN109273355B CN201810626521.6A CN201810626521A CN109273355B CN 109273355 B CN109273355 B CN 109273355B CN 201810626521 A CN201810626521 A CN 201810626521A CN 109273355 B CN109273355 B CN 109273355B
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selenium
sheet
switch
furnace
aluminum plate
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CN109273355A (en
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钱林
陈晶
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Hebi Weida Kexun Electric Co ltd
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Hebi Weida Kexun Electric Co ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/06Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/06Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. 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
    • H01L21/10Preliminary treatment of the selenium or tellurium, its application to the foundation plate, or the subsequent treatment of the combination
    • H01L21/101Application of the selenium or tellurium to the foundation plate

Abstract

The invention discloses a preparation process of a selenium rectifying slice. The selenium fairing is prepared by the processes of slicing, washing, sand blasting, drying, bismuth evaporation, selenium preparation, selenium evaporation, back evaporation of slices, pre-energizing, punching and shearing, alloy melting, alloy spraying, sheet connection, main energizing, chamfering, impacting, electric energizing, impacting, screening, reverse measurement, finished inspection packaging and warehousing storage. The invention uses semiconductor selenium as main material, and applies selenium on the commutator by special process to form selenium semiconductor element, which enhances commutation and overload protection, prolongs the service life of semiconductor element, and achieves the purpose of energy saving and consumption reduction.

Description

Preparation process of selenium rectifying sheet
The technical field is as follows:
the invention relates to a preparation process of a selenium rectifier cell, which is widely used for rectification and overload protection of an industrial electronic and electrical system.
Background art:
selenium has photosensitivity and semiconductivity and is commonly used in the electronics industry to make photovoltaic cells, photoreceptors, laser devices, infrared controllers, phototubes, photoresistors, optics, photometers, rectifiers, and the like. The use of selenium in the electronics industry accounts for about 30% of the total demand. The selenium rectifier has the characteristics of load resistance, high temperature resistance, good electrical stability and the like.
The selenium rectifying sheet is a core part of a selenium stack, a surge absorber and a semiconductor rectifying element, and the function and the performance of the selenium rectifying sheet depend on the quality of raw materials and the process preparation process. The current commutator segment selenium adding process is still immature, and the process of coating selenium on the commutator segment is too simple, so that the commutation and overload protection of the semiconductor element are too low, and the service life of the semiconductor element is shortened.
The invention content is as follows:
the invention aims to solve the technical problem of providing a preparation process of a selenium rectifying slice, which utilizes semiconductor selenium as a main material and adopts a special process to coat the selenium on a rectifying slice to form a selenium slice semiconductor element, thereby enhancing the rectification and overload protection, prolonging the service life of the semiconductor element and achieving the purposes of saving energy and reducing consumption.
The technical scheme adopted by the invention for solving the technical problem is as follows: a selenium fairing of selenium fairing preparation technology is prepared by slicing, washing, sand blasting, drying, bismuth evaporation, selenium preparation, selenium evaporation, back evaporation of the fairing, pre-energizing, punching and shearing, alloy melting, alloy spraying, connection of the fairing, main energizing, chamfering, impact, electric energizing, impact, screening, reverse measurement, quality inspection, packaging and warehousing storage technology, and the specific preparation process comprises the following steps:
(1) the slicing step comprises the following steps: cutting a large aluminum plate into the sizes of 0.8mm multiplied by 1015mm multiplied by 2040mm, strictly preventing scratching the surface in the material cutting process, wherein an oxidized layer on the surface of the aluminum plate can not be cut, and the large aluminum plate can not be cut if mechanical hard damage exists before cutting;
(2) the film washing: firstly, scrubbing greasy dirt on the surface of the aluminum plate by using gasoline, then scrubbing the greasy dirt on the surface of the aluminum plate by using alkaline water, wherein the scrubbed surface of the aluminum plate is bright and free of dirt, and the scratch area of the aluminum plate is more than or equal to 10mm2If the product is to be removed, the product is not allowed to flow into the next procedure;
(3) the sand blasting: the operation process is as follows: firstly, switching on a power supply of a dust remover, pouring quartz sand into a cabin, adding 60kg of sand every time, adding the sand 4 times in the whole working time, wherein 15kg of sand is not poured once every time, then checking a nozzle, switching on a power supply of a linkage mechanism of a sand blasting machine, opening a compressed air valve, and stabilizing the air pressure within the range of 68.647-88.620 KPa, namely blasting sand; guiding the aluminum plate subjected to sand blasting into a sand blasting wheel, taking down the aluminum plate, and finally identifying the surface, wherein the aluminum plate is light gray after sand blasting, the surface cannot have serious black marks and light spots, and if the aluminum plate has bright light, the aluminum plate needs to be re-sprayed at the air pressure of 39.227-88.260 KPa once;
(4) and (3) drying: the operation process is as follows: and vertically loading the aluminum plate into a drying vehicle, turning on a main switch and a blower, and switching on all switches for heating 12 KW. Pushing a drying vehicle provided with an aluminum plate into a furnace, preheating the furnace before working, closing a furnace door, heating the furnace to 175 +/-5 ℃ within 15 minutes, preserving the temperature for 2 hours, properly heating by 4KW or 2KW after reaching the temperature, keeping the temperature, disconnecting a heating switch, closing an air blower, disconnecting a main switch and pulling out a loading vehicle after drying is finished; naturally cooling the dried aluminum plate for 10-15 minutes, putting the aluminum plate into a chip loading vehicle, keeping the aluminum plate in a drying furnace for more than 4 hours, keeping the aluminum plate in the drying furnace for more than 4 hours, and drying the aluminum plate again for 30 minutes at the temperature of 100-120 ℃ when the chip storage time is more than 24 hours;
(5) the evaporation of bismuth: the operation process is as follows: opening a ventilation valve of the bismuth pot, dropping the vacuum pot, inserting a safety pin, stacking frames containing less than or equal to 20 aluminum plates on a storage rack, adding a cover plate, hanging a support welding block, and placing the small bismuth pot into a furnace according to the number, wherein the weight of bismuth in each pot is 45g +/-1 g;
the bismuth evaporation process comprises the steps of closing a large pre-vacuum pump inlet air valve, starting a large pre-vacuum pump, opening a large pre-pump pot valve, opening a diffusion pump pot valve when the vacuum degree reaches 2.666Pa, closing the large pre-pump vacuum valve, connecting the large pre-pump vacuum valve with a diffusion pump in parallel at any time, opening the large pre-pump inlet air valve, closing the large pre-pump and cooling water, and adjusting an aluminum plate counter; switching on a heating switch of a bismuth pot when the vacuum degree reaches 1.666Pa, automatically evaporating after heating for 15 minutes, adjusting the evaporation time to 2-4 minutes, adjusting the power of the bismuth pot according to the bismuth layer of the previous pot, recording the vacuum degree of evaporating the first, middle and last bismuth sheets, sounding the last sound annunciator after evaporating, closing the sound annunciator switch, a diffusion pump valve and a heating power supply, opening a ventilation valve after thirty minutes, falling down a vacuum pot, disengaging a rotating clutch, taking down a baffle block, taking out the evaporated bismuth sheets, putting the bismuth sheets into a sheet loading vehicle, and sending selenium for evaporation after the bismuth sheets are qualified; the bismuth sheet is stored in the product for less than or equal to 6 hours, and no trace mercury vapor, various oils and volatile substances are allowed to be stored indoors, so that scratches, mechanical damage, oil stains and fingerprints cannot be caused on the aluminum plate, and the aluminum plate cannot be deformed;
(6) the preparation of the selenium comprises the following steps: the operation process is as follows: weighing two parts of 70g selenium powder by using a balance, pouring one part of the selenium powder into a ground triangular beaker, measuring 15ml of liquid bromine by using a measuring cylinder, pouring the liquid bromine into the triangular flask, slowly and continuously shaking the liquid bromine at the speed of pouring, slowly pouring the other part of the 70ml selenium powder in the beaker into a triangular flask by shaking, then covering a cover, and storing for 48 hours to prepare selenium addition;
adding selenium, weighing 5kg of selenium, pouring the selenium into a stainless steel stirring pot, heating and melting, stirring for 2 hours at 300-350 ℃, clamping a triangular flask mouth filled with selenium bromide by using a clamp, melting on an electric furnace, pouring the selenium into the stirred selenium, continuously stirring for 5 minutes when the selenium is cooled to 290 ℃, respectively pouring the selenium solution into an aluminum tray after the selenium solution is cooled to 240-250 ℃, respectively sampling from the first tray, the middle tray and the last tray, mixing and grinding the selenium solution into two parts, analyzing the bromine content, controlling the bromine content to be generally 1%, grinding the added selenium into small blocks with the diameter of less than 10mm by using a mortar, filling the small blocks into a black ground bottle with a cover, and storing the small blocks in a cool dark cabinet;
(7) the evaporation of selenium: the operation process is as follows: opening cooling water → an operation panel bus bar → an aluminum sheet heating power supply for preheating for 1.5 h-2.5 h → a selenium furnace heating power supply, opening a ventilation valve after 30 minutes, dropping a vacuum pan, wherein the temperature of the selenium furnace is 280-300 ℃, closing the aluminum sheet heating power supply → operating a charging switch, driving the selenium furnace to a charging position, charging selenium into a furnace groove until the selenium is 0.8cm, pushing a weighed aluminum plate into a plug sheet groove with the bismuth surface facing downwards, installing an aluminum plate cover, operating a furnace shutdown switch, driving the selenium furnace to a parking position, closing the vacuum pan by using compressed air, and opening the vacuum power supply;
(8) the steaming back sheet: the operation process is as follows: the evaporation process comprises the steps of opening a valve of a large pre-vacuum pump after the vacuum pump starts to work, vacuumizing for 10-20 minutes, opening an aluminum skin heating power supply, heating for 3-4 minutes with the heating power of 1.5KW, and waiting for the vacuum degree to reach 8Pa6 multiplied by 10-2When the evaporation time is 12-15 minutes, the furnace car is driven to a stop position. The weight of the selenium layer is 90-130 g, the weight error is less than or equal to 3%, an air inlet valve is opened, a large pre-vacuum pump is closed, a vacuum pan falls down, a safety pin is inserted, a front end cover of an aluminum sheet is taken out, a selenium sheet is clamped by a flat jaw, the jaw clamping sheet is 5mm, the weight of selenium is weighed, the sheet is vertically placed into a sheet loading vehicle, the weight is filled for recording, the continuous evaporation time is less than or equal to 4 minutes, the reworked selenium sheet is evaporated within 4 hours after pre-energizing, the twice evaporation weight is 90-130 g, no trace mercury vapor is allowed in a room, and the pre-energizing interval time is less than or equal to 48 hours;
(9) the pre-energizing: the operation process is as follows: firstly, turning on a power switch and a motor switch, turning on 6KW, 4KW and 2KW, vertically inserting selenium sheets steamed with selenium into an energizing vehicle, correspondingly loading selenium surfaces, placing a lining on each vehicle, then loading the selenium sheets with the quantity less than or equal to 30 sheets, after the furnace temperature reaches 110 ℃, opening a furnace door, paving rails of the energizing vehicle, pushing the energizing vehicle into the energizing vehicle, closing the furnace door, raising the furnace temperature to 104 ℃, turning off a 6KW and 4KW heating switch, controlling the 2KW or 4KW by using a contact thermometer when the furnace temperature rises to 112 +/-2 ℃ due to inertia, keeping the temperature for 2 hours, pulling out the furnace vehicle after the motor switch and the power switch are turned off, cooling for 10-15 minutes, then extracting the selenium sheets and loading the selenium sheets into a sheet storage vehicle, and allowing no trace mercury vapor in a room;
(10) the punching and shearing: the operation process is as follows: checking whether each part of the machine tool is normal, soaking clean cotton yarn in alcohol to wipe scissors and a working table, pressing a black button, starting a shearing machine, putting a long selenium sheet into a die according to a specified size, and punching on a punch press to obtain a qualified selenium sheet
Figure BSA0000165631420000051
152、222、302、402The selenium sheet or the connection sheet is punched and cut into connection sheets, the connection sheets are put into a certain die after being energized, and then the connection sheets are punched into qualified single sheets;
(11) the fusion gold: the operation process is as follows: weighing 10-15 kg of tin, cadmium and thallium used in the alloy production process according to the weight of thallium g (68% of tin + 32% of cadmium) 2/ten thousand, wiping off an aluminum alloy pot, putting the weighed tin into the pot, opening an electric heating switch, heating the tin to 350 ℃, adding weighed cadmium when cooling to 220-240 ℃, opening a ventilation cabinet, keeping the temperature and stirring for 30 minutes when the temperature rises to 240 +/-10 ℃ after dissolving, taking out surface scum with a scoop, adding the weighed thallium into the tin-cadmium alloy, keeping the temperature of 240 +/-10 ℃ and stirring for 30 minutes, taking out the surface scum with the scoop, injecting alloy liquid into a mold, and closing the electric heating switch and the ventilation cabinet;
(12) the alloy spraying and sheet connecting step: the operation process is as follows: putting the alloy strip into a melting pot, turning on a heating switch of an electric furnace, controlling by a thermocouple thermometer when the temperature reaches 240 +/-10 ℃ after the ternary alloy is melted, turning on a spray gun heating power supply 25 minutes before operation, and properly adjusting the heating power supply; then the cabinet is put in a loading way,
Figure BSA0000165631420000054
Figure BSA0000165631420000055
the selenium sheet is upward and placed on the bottom plate, and the covering button is arranged; the 60 x 60 selenium sheet is upwards placed on the bottom plate, the covering button is arranged in the inlet hole, the sample plate and the pressing frame are arranged, the clamp is tightened, the alloy is injected into the spray gun by the spoon, and the air draft power supply and the air compressor power supply are turned on; the alloy spraying frame is put into a spray gun, and the air pressure is adjusted to be 4 plus or minus 0.2kg/cm2,Uniformly spraying alloy on the spray gun head which is 8 +/-1.5 cm away from the selenium sheet, and taking out the sprayed selenium sheet for sheet connection;
(13) the main enabling comprises the following steps: the operation process is as follows: preheating an 8KW furnace 3 days in advance, protecting the furnace temperature by using a contact thermometer at 217 +/-5 ℃, starting transfer, adjusting a transformer, controlling the main energization time to be 26-40 minutes, putting a selenium sheet on the inlet of a conveyor belt in a downward mode, starting main energization of a naphthalene feeding furnace, taking down the selenium sheet at the outlet, predicting the same direction and the reverse direction, sending the selenium sheet according to requirements, taking out all commutator segments, and turning off the power supply of a conveying motor;
(14) chamfering the selenium sheet: the operation process is as follows: placing the prepared selenium sheet in a positioning hole, switching on a power switch, switching on a button switch, rotating a motor, correcting the depth of the turning tool again according to the selenium sheet chamfered at the first part until the selenium sheet is qualified, ensuring that the chamfer size of the circumference of the selenium sheet is within 0.2 multiplied by 20 degrees to 45 degrees, taking 5-10 sheets for inspection and identification, producing the selenium sheet after the chamfer quality is qualified, ejecting the poured selenium sheet into a material receiving box by an automatic spring, and after the operation is finished, switching off the power supply of the motor, and delivering the selenium sheet to a main power supply;
(15) the impact is as follows: the operation process is as follows: and turning on a power switch C, namely turning on a 100 muf indicator light, pressing a contact voltage into a short circuit indicator light, putting the selenium sheet alloy surface upwards on the contact electrode, adding 40V voltage, pressing the contact electrode, if the short circuit indicator light is not on, the selenium sheet is qualified, otherwise, if the selenium sheet is short-circuited, the capacitance impact is increased. If the short-circuit indicator lamp is still on when the C is 500 muf impact, 50V, 60V and 70V impact is added, the short-circuit indicator lamp is still on and scrapped, the contact electrodes are pressed and short-circuited, the capacitor is discharged, the modulator is reset to zero, and the power switch is switched off;
(16) the electric energizing and impact sieve sheet comprises: the operation process is as follows: inserting a commutator segment between energizing electrodes on the reverse side of an energizing instrument, enabling alloy surfaces to face the same direction, checking whether switches of all parts of the energizing instrument are placed at correct positions, adjusting work according to the room temperature condition, enabling a time-of-rest relay to be normal to guarantee energizing requirements, turning on a main power switch of an energizing table, turning on a starting button switch, continuously working a switch, adjusting energizing voltage, turning on a shunt energizing switch, turning on a shunt short-circuit current adjusting switch to a short-circuit position, immediately adjusting a variable resistor, turning the shunt short-circuit switch to the energizing position, taking off a selenium commutator segment, storing for 24 hours, then carrying out impact test operation, and screening the selenium commutator segments qualified in the impact test;
(17) the reverse measurement is as follows: the operation process is as follows: wearing a rubber finger, taking out the screened qualified selenium sheets, selecting a measuring table according to the sheet type, checking an instrument of the measuring table, switching on a stabilized voltage supply switch and a measuring table switch after the proof of certification is verified, turning on a power supply switch, adjusting the measuring voltage according to a sorting method specified by the measuring table, enabling the alloy surface of the selenium rectifying sheet to face upwards, switching on a test pen for 5 seconds, judging whether the current reading is in a qualified range, switching off the power supply and the stabilized voltage supply after the measurement is finished, switching to the measurement of the measured qualified products, and continuing to electrify the unqualified products;
(18) leading to the measurement: the operation process is as follows: and selecting a measuring table according to the sheet type, wearing a rubber finger, taking out the selenium sheet, switching on a stabilized voltage supply switch and a measuring table switch after checking that the measuring table is qualified and effective, switching on a test meter pen when the alloy surface of the measuring sheet faces upwards, and regulating the current to a rated value. Adjusting current, measuring voltage, closing a switch of a measuring table and a switch of a voltage-stabilized power supply, placing selenium sheets in a specified box according to grouping requirements, and assembling or packaging after the selenium sheets are qualified to be detected;
(19) packaging the finished product, and warehousing for storage: after the finished product is inspected to be qualified, the number of the packaged pieces is 152~402: each bag containing 200 tablets, 602~1002: each bag contains 50 sheets, and is wrapped with a layer of damp-proof paper, then a layer of kraft paper, and the kraft paper is coated with selenium sheetsThe type, the seal of red printing oil, the seal of year, month and day, the type, the group, the quantity and the seal of blue printing for the selenium sheet are taken out of the factory and finally stored in a warehouse.
The invention has the beneficial effects that: because semiconductor selenium is used as a main material, selenium is coated on the rectifier sheet by adopting a special process to form the selenium sheet semiconductor element, the rectification and overload protection are enhanced, the service life of the semiconductor element is prolonged, and the purposes of energy conservation and consumption reduction are achieved, thereby realizing the requirements of high quality and light weight of an electronic and electrical system.
Description of the drawings:
FIG. 1 is a process flow diagram of the present invention.
The specific implementation mode is as follows:
example 1: as shown in fig. 1, the selenium fairing of the selenium fairing preparation process is prepared by slicing, washing, sand blasting, drying, bismuth evaporation, selenium preparation, selenium evaporation, back evaporation of the selenium fairing, pre-energizing, punching and shearing, alloy melting, alloy spraying, jointing, main energizing, chamfering, impacting, electric energizing, impacting, screening, reverse measurement, finished inspection packaging and warehousing storage processes, and the specific process preparation process comprises the following steps:
(1) the slicing step comprises the following steps: cutting a large aluminum plate into the sizes of 0.8mm multiplied by 1015mm multiplied by 2040mm, strictly preventing scratching the surface in the material cutting process, wherein an oxidized layer on the surface of the aluminum plate can not be cut, and the large aluminum plate can not be cut if mechanical hard damage exists before cutting;
(2) the film washing: firstly, scrubbing greasy dirt on the surface of the aluminum plate by using gasoline, then scrubbing the greasy dirt on the surface of the aluminum plate by using alkaline water, wherein the scrubbed surface of the aluminum plate is bright and free of dirt, and the scratch area of the aluminum plate is more than or equal to 10mm2If the product is to be removed, the product is not allowed to flow into the next procedure;
(3) the sand blasting: the operation process is as follows: firstly, switching on a power supply of a dust remover, pouring quartz sand into a cabin, adding 60kg of sand every time, adding the sand 4 times in the whole working time, wherein 15kg of sand is not poured once every time, then checking a nozzle, switching on a power supply of a linkage mechanism of a sand blasting machine, opening a compressed air valve, and stabilizing the air pressure within the range of 68.647-88.620 KPa, namely blasting sand; guiding the aluminum plate subjected to sand blasting into a sand blasting wheel, taking down the aluminum plate, and finally identifying the surface, wherein the aluminum plate is light gray after sand blasting, the surface cannot have serious black marks and light spots, and if the aluminum plate has bright light, the aluminum plate needs to be re-sprayed at the air pressure of 39.227-88.260 KPa once;
(4) and (3) drying: the operation process is as follows: and vertically loading the aluminum plate into a drying vehicle, turning on a main switch and a blower, and switching on all switches for heating 12 KW. Pushing a drying vehicle provided with an aluminum plate into a furnace, preheating the furnace before working, closing a furnace door, heating the furnace to 175 +/-5 ℃ within 15 minutes, preserving the temperature for 2 hours, properly heating by 4KW or 2KW after reaching the temperature, keeping the temperature, disconnecting a heating switch, closing an air blower, disconnecting a main switch and pulling out a loading vehicle after drying is finished; naturally cooling the dried aluminum plate for 10-15 minutes, putting the aluminum plate into a chip loading vehicle, keeping the aluminum plate in a drying furnace for more than 4 hours, keeping the aluminum plate in the drying furnace for more than 4 hours, and drying the aluminum plate again for 30 minutes at the temperature of 100-120 ℃ when the chip storage time is more than 24 hours;
(5) the evaporation of bismuth: the operation process is as follows: opening a ventilation valve of the bismuth pot, dropping the vacuum pot, inserting a safety pin, stacking frames containing less than or equal to 20 aluminum plates on a storage rack, adding a cover plate, hanging a support welding block, and placing the small bismuth pot into a furnace according to the number, wherein the weight of bismuth in each pot is 45g +/-1 g;
the bismuth evaporation process comprises the steps of closing a large pre-vacuum pump inlet air valve, starting a large pre-vacuum pump, opening a large pre-pump pot valve, opening a diffusion pump pot valve when the vacuum degree reaches 2.666Pa, closing the large pre-pump vacuum valve, connecting the large pre-pump vacuum valve with a diffusion pump in parallel at any time, opening the large pre-pump inlet air valve, closing the large pre-pump and cooling water, and adjusting an aluminum plate counter; switching on a heating switch of a bismuth pot when the vacuum degree reaches 0.666Pa, automatically evaporating after heating for 15 minutes, adjusting the evaporation time to 2-4 minutes, adjusting the power of the bismuth pot according to the bismuth layer of the previous pot, recording the vacuum degree of evaporating the first, middle and last bismuth sheets, sounding the last sound annunciator after evaporating, closing the sound annunciator switch, a diffusion pump valve and a heating power supply, opening a ventilation valve after thirty minutes, falling down a vacuum pot, disengaging a rotating clutch, taking down a baffle block, taking out the evaporated bismuth sheets, putting the bismuth sheets into a sheet loading vehicle, and sending selenium for evaporation after the bismuth sheets are qualified; the bismuth sheet is stored in the product for less than or equal to 6 hours, and no trace mercury vapor, various oils and volatile substances are allowed to be stored indoors, so that scratches, mechanical damage, oil stains and fingerprints cannot be caused on the aluminum plate, and the aluminum plate cannot be deformed;
(6) the preparation of the selenium comprises the following steps: the operation process is as follows: weighing two parts of 70g selenium powder by using a balance, pouring one part of the selenium powder into a ground triangular beaker, measuring 15ml of liquid bromine by using a measuring cylinder, pouring the liquid bromine into the triangular flask, slowly and continuously shaking the liquid bromine at the speed of pouring, slowly pouring the other part of the 70ml selenium powder in the beaker into a triangular flask by shaking, then covering a cover, and storing for 48 hours to prepare selenium addition;
adding selenium, weighing 5kg of selenium, pouring the selenium into a stainless steel stirring pot, heating and melting, stirring for 2 hours at 300-350 ℃, clamping a triangular flask mouth filled with selenium bromide by using a clamp, melting on an electric furnace, pouring the selenium into the stirred selenium, continuously stirring for 5 minutes when the selenium is cooled to 290 ℃, respectively pouring the selenium solution into an aluminum tray after the selenium solution is cooled to 240-250 ℃, respectively sampling from the first tray, the middle tray and the last tray, mixing and grinding the selenium solution into two parts, analyzing the bromine content, controlling the bromine content to be generally 1%, grinding the added selenium into small blocks with the diameter of less than 10mm by using a mortar, filling the small blocks into a black ground bottle with a cover, and storing the small blocks in a cool dark cabinet;
(7) the evaporation of selenium: the operation process is as follows: opening cooling water → an operation panel bus bar → an aluminum sheet heating power supply for preheating for 1.5 h-2.5 h → a selenium furnace heating power supply, opening a ventilation valve after 30 minutes, dropping a vacuum pan, wherein the temperature of the selenium furnace is 280-300 ℃, closing the aluminum sheet heating power supply → operating a charging switch, driving the selenium furnace to a charging position, charging selenium into a furnace groove until the selenium is 0.8cm, pushing a weighed aluminum plate into a plug sheet groove with the bismuth surface facing downwards, installing an aluminum plate cover, operating a furnace shutdown switch, driving the selenium furnace to a parking position, closing the vacuum pan by using compressed air, and opening the vacuum power supply;
(8) the steaming back sheet: the operation process is as follows: the evaporation process comprises the steps of opening a valve of a large pre-vacuum pump after the vacuum pump starts to work, vacuumizing for 10-20 minutes, opening an aluminum skin heating power supply, heating for 3-4 minutes with the heating power of 1.5KW, and waiting for the vacuum degree to reach 8Pa6 multiplied by 10-2When the evaporation time is 12-15 min, the furnace carriage is driven to turn on the power supply of the furnace carriage, the aluminum sheet is turned off to heat, evaporation is started, and the furnace carriage is turned on after the specified evaporation time is reached, wherein the evaporation time is 12-15 minAnd driving to a parking place. The weight of the selenium layer is 90-130 g, the weight error is less than or equal to 3%, an air inlet valve is opened, a large pre-vacuum pump is closed, a vacuum pan falls down, a safety pin is inserted, a front end cover of an aluminum sheet is taken out, a selenium sheet is clamped by a flat jaw, the jaw clamping sheet is 5mm, the weight of selenium is weighed, the sheet is vertically placed into a sheet loading vehicle, the weight is filled for recording, the continuous evaporation time is less than or equal to 4 minutes, the reworked selenium sheet is evaporated within 4 hours after pre-energizing, the twice evaporation weight is 90-130 g, no trace mercury vapor is allowed in a room, and the pre-energizing interval time is less than or equal to 48 hours;
(9) the pre-energizing: the operation process is as follows: firstly, turning on a power switch and a motor switch, turning on 6KW, 4KW and 2KW, vertically inserting selenium sheets steamed with selenium into an energizing vehicle, correspondingly loading selenium surfaces, placing a lining on each vehicle, then loading the selenium sheets with the quantity less than or equal to 30 sheets, after the furnace temperature reaches 110 ℃, opening a furnace door, paving rails of the energizing vehicle, pushing the energizing vehicle into the energizing vehicle, closing the furnace door, raising the furnace temperature to 104 ℃, turning off a 6KW and 4KW heating switch, controlling the 2KW or 4KW by using a contact thermometer when the furnace temperature rises to 112 +/-2 ℃ due to inertia, keeping the temperature for 2 hours, pulling out the furnace vehicle after the motor switch and the power switch are turned off, cooling for 10-15 minutes, then extracting the selenium sheets and loading the selenium sheets into a sheet storage vehicle, and allowing no trace mercury vapor in a room;
(10) the punching and shearing: the operation process is as follows: checking whether each part of the machine tool is normal, soaking clean cotton yarn in alcohol to wipe scissors and a working table, pressing a black button, starting a shearing machine, putting a long selenium sheet into a die according to a specified size, and punching on a punch press to obtain a qualified selenium sheet
Figure BSA0000165631420000111
152、222、302、402The selenium sheet or the connection sheet is punched and cut into connection sheets, the connection sheets are put into a certain die after being energized, and then the connection sheets are punched into qualified single sheets;
(11) the fusion gold: the operation process is as follows: weighing 10-15 kg of tin, cadmium and thallium used in the alloy production process according to the weight of thallium g (68% of tin + 32% of cadmium) 2/ten thousand, wiping off an aluminum alloy pot, putting the weighed tin into the pot, opening an electric heating switch, heating the tin to 350 ℃, adding weighed cadmium when cooling to 220-240 ℃, opening a ventilation cabinet, keeping the temperature and stirring for 30 minutes when the temperature rises to 240 +/-10 ℃ after dissolving, taking out surface scum with a scoop, adding the weighed thallium into the tin-cadmium alloy, keeping the temperature of 240 +/-10 ℃ and stirring for 30 minutes, taking out the surface scum with the scoop, injecting alloy liquid into a mold, and closing the electric heating switch and the ventilation cabinet;
(12) the alloy spraying and sheet connecting step: the operation process is as follows: putting the alloy strip into a melting pot, turning on a heating switch of an electric furnace, controlling by a thermocouple thermometer when the temperature reaches 240 +/-10 ℃ after the ternary alloy is melted, turning on a spray gun heating power supply 25 minutes before operation, and properly adjusting the heating power supply; then the cabinet is put in a loading way,
Figure BSA0000165631420000114
Figure BSA0000165631420000115
the selenium sheet is upward and placed on the bottom plate, and the covering button is arranged; the 60 x 60 selenium sheet is upwards placed on the bottom plate, the covering button is arranged in the inlet hole, the sample plate and the pressing frame are arranged, the clamp is tightened, the alloy is injected into the spray gun by the spoon, and the air draft power supply and the air compressor power supply are turned on; the alloy spraying frame is put into a spray gun, and the air pressure is adjusted to be 4 plus or minus 0.2kg/cm2,Uniformly spraying alloy on the spray gun head which is 8 +/-0.5 cm away from the selenium sheet, and taking out the sprayed selenium sheet for sheet connection;
(13) the main enabling comprises the following steps: the operation process is as follows: preheating an 8KW furnace 3 days in advance, protecting the furnace temperature by using a contact thermometer at 217 +/-5 ℃, starting transfer, adjusting a transformer, controlling the main energization time to be 26-40 minutes, putting a selenium sheet on the inlet of a conveyor belt in a downward mode, starting main energization of a naphthalene feeding furnace, taking down the selenium sheet at the outlet, predicting the same direction and the reverse direction, sending the selenium sheet according to requirements, taking out all commutator segments, and turning off the power supply of a conveying motor;
(14) chamfering the selenium sheet: the operation process is as follows: placing the prepared selenium sheet in a positioning hole, switching on a power switch, switching on a button switch, rotating a motor, correcting the depth of the turning tool again according to the selenium sheet chamfered at the first part until the selenium sheet is qualified, ensuring that the chamfer size of the circumference of the selenium sheet is within 0.2 multiplied by 20 degrees to 45 degrees, taking 5-10 sheets for inspection and identification, producing the selenium sheet after the chamfer quality is qualified, ejecting the poured selenium sheet into a material receiving box by an automatic spring, and after the operation is finished, switching off the power supply of the motor, and delivering the selenium sheet to a main power supply;
(15) the impact is as follows: the operation process is as follows: and turning on a power switch C, namely turning on a 100 muf indicator light, pressing a contact voltage into a short circuit indicator light, putting the selenium sheet alloy surface upwards on the contact electrode, adding 40V voltage, pressing the contact electrode, if the short circuit indicator light is not on, the selenium sheet is qualified, otherwise, if the selenium sheet is short-circuited, the capacitance impact is increased. If the short-circuit indicator lamp is still on when the C is 500 muf impact, 50V, 60V and 70V impact is added, the short-circuit indicator lamp is still on and scrapped, the contact electrodes are pressed and short-circuited, the capacitor is discharged, the modulator is reset to zero, and the power switch is switched off;
(16) the electric energizing and impact sieve sheet comprises: the operation process is as follows: inserting a commutator segment between energizing electrodes on the reverse side of an energizing instrument, enabling alloy surfaces to face the same direction, checking whether switches of all parts of the energizing instrument are placed at correct positions, adjusting work according to the room temperature condition, enabling a time-of-rest relay to be normal to guarantee energizing requirements, turning on a main power switch of an energizing table, turning on a starting button switch, continuously working a switch, adjusting energizing voltage, turning on a shunt energizing switch, turning on a shunt short-circuit current adjusting switch to a short-circuit position, immediately adjusting a variable resistor, turning the shunt short-circuit switch to the energizing position, taking off a selenium commutator segment, storing for 24 hours, then carrying out impact test operation, and screening the selenium commutator segments qualified in the impact test;
(17) the reverse measurement is as follows: the operation process is as follows: wearing a rubber finger, taking out the screened qualified selenium sheets, selecting a measuring table according to the sheet type, checking an instrument of the measuring table, switching on a stabilized voltage supply switch and a measuring table switch after the proof of certification is verified, turning on a power supply switch, adjusting the measuring voltage according to a sorting method specified by the measuring table, enabling the alloy surface of the selenium rectifying sheet to face upwards, switching on a test pen for 5 seconds, judging whether the current reading is in a qualified range, switching off the power supply and the stabilized voltage supply after the measurement is finished, switching to the measurement of the measured qualified products, and continuing to electrify the unqualified products;
(18) leading to the measurement: the operation process is as follows: and selecting a measuring table according to the sheet type, wearing a rubber finger, taking out the selenium sheet, switching on a stabilized voltage supply switch and a measuring table switch after checking that the measuring table is qualified and effective, switching on a test meter pen when the alloy surface of the measuring sheet faces upwards, and regulating the current to a rated value. Adjusting current, measuring voltage, closing a switch of a measuring table and a switch of a voltage-stabilized power supply, placing selenium sheets in a specified box according to grouping requirements, and assembling or packaging after the selenium sheets are qualified to be detected;
(19) packaging the finished product, and warehousing for storage: after the finished product is inspected to be qualified, the number of the packaged pieces is 152~402: each bag containing 200 tablets, 602~1002: and each package of 50 selenium sheets is firstly wrapped with a layer of damp-proof paper, then wrapped with a layer of kraft paper, printed with selenium sheet specifications, types and red printing oil stamps, and the selenium sheets are individually subjected to blue printing for classification, group, quantity and year, month and day stamps before being delivered to a factory and finally stored in a warehouse.
Example 2: as shown in fig. 1, in the (6) selenium preparing and producing process of the selenium fairing preparation process, the selenium preparation process comprises the following steps: weighing selenium to be prepared, pouring the selenium into a stainless steel selenium pot, heating and melting the selenium to 300-350 ℃, stirring for 2-8 hours, cooling to 290 ℃, removing scum on the surface of the selenium, adding weighed added selenium, continuously stirring, stirring for 10-40 kg of selenium for 10-20 minutes, calculating the amount of the added selenium according to the weight of the actually produced selenium in the pot, cooling to 240-250 ℃, pouring the selenium into aluminum trays respectively, pouring the selenium which is black, quickly pouring the selenium, avoiding the selenium from falling out at a low temperature, sampling the prepared selenium from the first tray, the middle tray and the last tray respectively, mixing and grinding the selenium into two parts, analyzing the bromine content of the two parts, packing the rest of selenium in boxes, numbering and placing the selenium racks in a specified amount, wherein the bromine content of the selenium generally does not exceed +/-20 percent of the specified amount, and evaporating the selenium is used according to qualified notice.
Example 3: as shown in fig. 1, the process for preparing a selenium rectifying tablet 4. the process for preparing a selenium finishing tablet according to claim 1 is characterized in that: in the (6) selenium preparation process, the adding weight to be added into the produced selenium is calculated according to the analysis result of bromine content of the added selenium;
calculating the public a ═ B × A/C
a- -weight of selenium required to be added
B- -selenium content required for production
A- - - -the weight of selenium powder filled in the stirring pot
C- -average bromine content in the added selenium.
As shown in fig. 1, in (6) the preparation process of the selenium current rectifier comprises the following steps: 2-5 g of production selenium and 1-2 g of added selenium are respectively taken out of analysis samples and put into a glass mortar to be ground into powder. Taking the ground selenium powder by using a horn spoon, and weighing 1-5 g on a precision balance; pouring the weighed selenium powder into a cleaned and dried triangular flask with the capacity of 500 ml;
dripping a pre-measured silver nitrate solution of 0.01N into a triangular flask by using an acid dropping pipe to generally produce 12-15 ml of selenium drops, and adding 20-25 ml of selenium drops; weighing 50ml of silver nitrate by using a measuring cylinder, and pouring into a triangular flask; putting a triangular flask containing silver nitrate and nitric acid samples into a water bath kettle, and heating at a low temperature, wherein the temperature of the water bath kettle is about 100 ℃;
during the selenium dissolving process, a large amount of nitrogen dioxide gas is generated, after the nitrogen dioxide gas is completely volatilized and the selenium is completely dissolved, the triangular flask is immediately taken down, the outer wall is washed by tap water, the temperature is substantially cooled to the room temperature, and water is absolutely prohibited from dripping into the flask; weighing 5ml of toluene, pouring into a triangular flask, weighing 5ml of saturated ammonium ferric alum solution, and pouring into the triangular flask; and measuring 0.01N of ammonium sulfate solution by using an acid burette for titration, wherein in the titration process, the excessive silver nitrate solution in the triangular flask is transparent at first and slightly greenish and then is milky white liquid until the silver nitrate solution is slightly reddish, uniformly shaking the silver nitrate solution until the silver nitrate solution is slightly reddish, and finally recording the data ml of the titrated ammonium thiocyanate.
Example 4: as shown in fig. 1, in the selenium preparing process of (6), the solution preparation and calibration are as follows:
in the preparation process, 0.7612gAR ammonium thiocyanate is weighed by a balance and is put into a 1000ml narrow-mouth bottle, distilled water is added to dilute the solution to 1000ml, and the solution is shaken uniformly;
during calibration, 0.0400g of metallic silver (accuracy: 0.0001g) was weighed by a precision balance and placed in a 300ml Erlenmeyer flaskIn the solution, 10ml of 1: 1HNO is added3Shaking to dissolve silver, heating on electric furnace to dissolve silver completely, stopping heating when nitrogen dioxide gas is volatilized, cooling, washing bottle wall with distilled water and diluting to 100ml, shaking uniformly, adding saturated ferric ammonium alum solution, immediately titrating with prepared ammonium thiocyanate, and shaking uniformly while dropping until brick red.
Calculating the formula: NH (NH)4CN5concentration-N
N=Ag(1g)/NH4CN5(ml)0.10788
The preparation process of the iron ammonium alum solution comprises the following steps:
cleaning and drying a container, weighing according to the solubility of ferric ammonium sulfate, wherein 100g of water is 44.15g at room temperature and 25 ℃, each time is about 500g, then putting the weighed solid ferric ammonium sulfate into distilled water, dissolving to light brown, titrating by using 1: 1 nitric acid until the brown disappears and becomes yellow green, and filtering the solution for use;
the preparation and calibration of the silver nitrate solution are as follows:
during preparation, 1.6989gAR silver nitrate is weighed by a balance, put into a 1000ml narrow-mouth bottle, added with a small amount of distilled water, dissolved, diluted with the distilled water to 1000ml and shaken uniformly;
during calibration, a newly prepared silver nitrate solution with a dropper is poured into a 300ml triangular flask, the solution is diluted by distilled water to about 100ml, 1ml of saturated ferric ammonium alum solution is added, ammonium thiocyanate solution with known concentration is added, the mixture is shaken while being dripped until red appears, and the reading is recorded;
calculating the formula: AgNO3Concentration N
N=NH4CNS(ML)×NH4CNS (concentration)/extraction AgNO3Volume ml.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (5)

1. A preparation process of a selenium rectifying slice is characterized by comprising the following steps: the selenium fairing is prepared by the processes of slicing, washing, sand blasting, drying, bismuth evaporation, selenium preparation, selenium evaporation, back evaporation of selenium slices, pre-energizing, punching and shearing, alloy melting, alloy spraying, sheet connection, main energizing, chamfering, impacting, electric energizing, impacting, screening, reverse measurement, finished inspection packaging and warehousing storage, and the specific process preparation process comprises the following steps:
(1) the slicing step comprises the following steps: cutting a large aluminum plate into the sizes of 0.8mm multiplied by 1015mm multiplied by 2040mm, strictly preventing scratching the surface in the material cutting process, wherein an oxidized layer on the surface of the aluminum plate can not be cut, and the large aluminum plate can not be cut if mechanical hard damage exists before cutting;
(2) the film washing: firstly, scrubbing oil stains on the surface of an aluminum plate by using gasoline, then scrubbing the oil stains on the surface of the aluminum plate by using alkaline water, wherein the scrubbed surface of the aluminum plate is bright and free of dirt, the scratch area of the aluminum plate is more than or equal to 10mm2, and the aluminum plate is removed and is not allowed to flow into the next procedure;
(3) the sand blasting: the operation process is as follows: firstly, switching on a power supply of a dust remover, pouring quartz sand into a cabin, adding 60kg of sand every time, adding the sand 4 times in the whole working time, wherein 15kg of sand is not poured once every time, then checking a nozzle, switching on a power supply of a linkage mechanism of a sand blasting machine, opening a compressed air valve, and stabilizing the air pressure within the range of 68.647-88.620 KPa, namely blasting sand; guiding the aluminum plate subjected to sand blasting into a sand blasting wheel, taking down the aluminum plate, and finally identifying the surface, wherein the aluminum plate is light gray after sand blasting, the surface cannot have serious black marks and light spots, and if the aluminum plate has bright light, the aluminum plate needs to be re-sprayed at the air pressure of 39.227-88.260 KPa once;
(4) and (3) drying: the operation process is as follows: vertically loading an aluminum plate into a drying vehicle, turning on a main switch and a blower, and switching on all switches for heating 12 KW; pushing a drying vehicle provided with an aluminum plate into a furnace, preheating the furnace before working, closing a furnace door, heating the furnace to 175 +/-5 ℃ within 15 minutes, preserving the temperature for 2 hours, properly heating by 4KW or 2KW after reaching the temperature, keeping the temperature, disconnecting a heating switch, closing an air blower, disconnecting a main switch and pulling out a loading vehicle after drying is finished; naturally cooling the dried aluminum plate for 10-15 minutes, putting the aluminum plate into a chip loading vehicle, keeping the time between the aluminum plate and bismuth evaporation for less than or equal to 4 hours and more than 4 hours in a drying furnace, keeping the aluminum plate for more than 24 hours, and drying the aluminum plate again for 30 minutes at the temperature of 100-120 ℃;
(5) the evaporation of bismuth: the operation process is as follows: opening a ventilation valve of the bismuth pot, dropping the vacuum pot, inserting a safety pin, stacking frames containing less than or equal to 20 aluminum plates on a storage rack, adding a cover plate, hanging a support welding block, and placing the small bismuth pot into a furnace according to the number, wherein the weight of bismuth in each pot is 45g +/-1 g;
the bismuth evaporation process comprises the steps of closing a large pre-vacuum pump inlet air valve, starting a large pre-vacuum pump, opening a large pre-pump pot valve, opening a diffusion pump pot valve when the vacuum degree reaches 2.666Pa, closing the large pre-pump vacuum valve, connecting the large pre-pump vacuum valve with a diffusion pump in parallel at any time, opening the large pre-pump inlet air valve, closing the large pre-pump and cooling water, and adjusting an aluminum plate counter; switching on a heating switch of a bismuth pot when the vacuum degree reaches 0.666Pa, automatically evaporating after heating for 15 minutes, adjusting the evaporation time to 2-4 minutes, adjusting the power of the bismuth pot according to the bismuth layer of the previous pot, recording the vacuum degree of evaporating the first, middle and last bismuth sheets, sounding the last sound annunciator after evaporating, closing the sound annunciator switch, a diffusion pump valve and a heating power supply, opening a ventilation valve after thirty minutes, falling down a vacuum pot, disengaging a rotating clutch, taking down a baffle block, taking out the evaporated bismuth sheets, putting the bismuth sheets into a sheet loading vehicle, and sending selenium for evaporation after the bismuth sheets are qualified; the bismuth sheet is stored in the product for less than or equal to 6 hours, and no trace mercury vapor, various oils and volatile substances are allowed to be stored indoors, so that scratches, mechanical damage, oil stains and fingerprints cannot be caused on the aluminum plate, and the aluminum plate cannot be deformed;
(6) preparing selenium: the operation process is as follows: weighing two parts of 70g selenium powder by using a balance, pouring one part of the selenium powder into a triangular beaker, measuring 15ml of liquid bromine by using a measuring cylinder, pouring the liquid bromine into the triangular beaker, slowly and continuously shaking the liquid bromine at a pouring speed, slowly pouring the other part of the 70g selenium powder into the triangular beaker by shaking, then covering a cover, and storing the liquid bromine for 48 hours to prepare selenium addition;
adding selenium, weighing 5kg of selenium, pouring the selenium into a stainless steel stirring pot, heating and melting, stirring for 2 hours at 300-350 ℃, clamping a triangular flask mouth filled with selenium bromide by using a clamp, melting on an electric furnace, pouring the selenium into the stirred selenium, continuously stirring for 5 minutes when the selenium is cooled to 290 ℃, respectively pouring the selenium solution into an aluminum tray after the selenium solution is cooled to 240-250 ℃, respectively sampling from the first tray, the middle tray and the last tray, mixing and grinding the selenium solution into two parts, analyzing the bromine content, controlling the bromine content to be 1%, grinding the added selenium into small blocks with the diameter of less than 10mm by using a mortar, filling the small blocks into a black ground bottle with a cover, and storing the small blocks in a cool dark cabinet;
(7) the evaporation of selenium: the operation process is as follows: opening cooling water → an operation panel bus bar → an aluminum sheet heating power supply for preheating for 1.5 h-2.5 h → a selenium furnace heating power supply, opening a ventilation valve after 30 minutes, dropping a vacuum pan, wherein the temperature of the selenium furnace is 280-300 ℃, closing the aluminum sheet heating power supply → operating a charging switch, driving the selenium furnace to a charging position, charging selenium into a furnace groove until the selenium is 0.8cm, pushing a weighed aluminum plate into a plug sheet groove with the bismuth surface facing downwards, installing an aluminum plate cover, operating a furnace shutdown switch, driving the selenium furnace to a parking position, closing the vacuum pan by using compressed air, and opening the vacuum power supply;
(8) the steaming back sheet: the operation process is as follows: the evaporation process is that after the vacuum pump starts to work, a valve of a large pre-vacuum pump is opened, after the vacuum pump is vacuumized for 10-20 minutes, an aluminum sheet heating power supply is opened, the heating is carried out for 3-4 minutes, the heating power is 1.5KW, when the vacuum degree reaches 8Pa6 multiplied by 10 < -2 >, an evaporation switch is operated, a furnace car power supply is switched on, the aluminum sheet heating is closed, evaporation is started, and after the specified evaporation time is reached, the furnace car is driven to a parking place after the evaporation time is 12-15 minutes; the weight of the selenium layer is 90-130 g, the weight error is less than or equal to 3%, an air inlet valve is opened, a large pre-vacuum pump is closed, a vacuum pan falls down, a safety pin is inserted, a front end cover of an aluminum sheet is taken out, a selenium sheet is clamped by a flat jaw, the jaw clamping sheet is 5mm, the weight of selenium is weighed, the sheet is vertically placed into a sheet loading vehicle, the weight is filled for recording, the continuous evaporation time is less than or equal to 4 minutes, the reworked selenium sheet is evaporated within 4 hours after pre-energizing, the twice evaporation weight is 90-130 g, no trace mercury vapor is allowed in a room, and the pre-energizing interval time is less than or equal to 48 hours;
(9) the pre-energizing: the operation process is as follows: firstly, turning on a power switch and a motor switch, turning on 6KW, 4KW and 2KW, vertically inserting selenium sheets steamed with selenium into an energizing vehicle, correspondingly loading selenium surfaces, placing a lining on each vehicle, then loading the selenium sheets with the quantity less than or equal to 30 sheets, after the furnace temperature reaches 110 ℃, opening a furnace door, paving rails of the energizing vehicle, pushing the energizing vehicle into the energizing vehicle, closing the furnace door, when the furnace temperature rises to 104 ℃, turning off a 6KW and 4KW heating switch, when the furnace temperature rises to 112 +/-2 ℃ due to inertia, controlling the 2KW or 4KW by using a contact thermometer, keeping the temperature for 2 hours, after the motor switch and the power switch are turned off, pulling out the furnace vehicle, after cooling for 10-15 minutes, extracting the selenium sheets and loading the selenium sheets into a sheet storage vehicle, wherein no trace mercury vapor is allowed in a room;
(10) the punching and shearing: the operation process is as follows: firstly, checking whether each part of a machine tool is normal, soaking alcohol in clean cotton yarn to wipe scissors and a workbench surface, pressing a black button, starting a shearing machine, putting a long selenium sheet into a die according to a specified size, punching the selenium sheet or a connection sheet into a punch press, punching the selenium sheet or the connection sheet into qualified phi 5, phi 7, 152, 222, 302 and 402, punching the punched connection sheet, putting the selenium sheet or the connection sheet into a certain die after main energization, and then punching the selenium sheet or the connection sheet into a qualified single sheet;
(11) the fusion gold: the operation process is as follows: weighing 10-15 kg of tin, cadmium and thallium used in the alloy production process according to the formula thallium g (68% of tin + 32% of cadmium)/2, wiping the aluminum alloy pot, putting the weighed tin into the pot, opening an electric heating switch, heating the tin to 350 ℃, adding the weighed cadmium when cooling to 220-240 ℃, opening a ventilation cabinet, keeping the temperature and stirring for 30 minutes when the temperature rises to 240 +/-10 ℃ after dissolving, taking out surface scum with a scoop, adding the weighed thallium into the tin-cadmium alloy, keeping the temperature to 240 +/-10 ℃ and stirring for 30 minutes, taking out the surface scum with the scoop, injecting alloy liquid into a mold, and closing the electric heating switch and the ventilation cabinet;
(12) the alloy spraying and sheet connecting step: the operation process is as follows: putting the alloy strip into a melting pot, turning on a heating switch of an electric furnace, controlling by a thermocouple thermometer when the temperature reaches 240 +/-10 ℃ after the ternary alloy is melted, turning on a spray gun heating power supply 25 minutes before operation, and properly adjusting the heating power supply; then, carrying out cabinet loading, enabling the phi 5-40 multiplied by 40 selenium sheets to face upwards, placing the selenium sheets on a bottom plate, and installing a covering button; the 60 x 60 selenium sheet is upwards placed on the bottom plate, the covering button is arranged in the inlet hole, the sample plate and the pressing frame are arranged, the clamp is tightened, the alloy is injected into the spray gun by the spoon, and the air draft power supply and the air compressor power supply are turned on; the alloy spraying frame is put into a spray gun, the air pressure is adjusted to 4 +/-0.2 kg/cm2, the distance between the spray gun head and the selenium sheet is 8 +/-0.5 cm, the alloy is uniformly sprayed, and the sprayed selenium sheet is taken out for sheet connection;
(13) the main enabling comprises the following steps: the operation process is as follows: preheating an 8KW furnace 3 days in advance, protecting the furnace temperature by using a contact thermometer at 217 +/-5 ℃, starting transfer, adjusting a transformer, controlling the main energization time to be 26-40 minutes, putting a selenium sheet on the inlet of a conveyor belt in a downward mode, starting main energization of a naphthalene feeding furnace, taking down the selenium sheet at the outlet, predicting the same direction and the reverse direction, sending the selenium sheet according to requirements, taking out all commutator segments, and turning off the power supply of a conveying motor;
(14) chamfering the selenium sheet: the operation process is as follows: placing the prepared selenium sheet in a positioning hole, switching on a power switch, switching on a button switch, rotating a motor, correcting the depth of the turning tool again according to the selenium sheet chamfered at the first part until the selenium sheet is qualified, ensuring that the chamfer size of the circumference of the selenium sheet is within 0.2 multiplied by 20 degrees to 45 degrees, taking 5-10 sheets for inspection and identification, producing the selenium sheet after the chamfer quality is qualified, ejecting the poured selenium sheet into a material receiving box by an automatic spring, and after the operation is finished, switching off the power supply of the motor, and delivering the selenium sheet for power supply;
(15) the impact is as follows: the operation process is as follows: turning on a power switch C-100 muf indicator light, pressing a contact voltage into a short circuit indicator light, putting the selenium sheet alloy surface upwards on a contact electrode, adding 40V voltage, pressing the contact electrode, if the short circuit indicator light is not on, the selenium sheet is qualified, otherwise, the selenium sheet is short-circuited, and capacitance impact is increased; if the short-circuit indicator lamp is still on when the C is 500 muf impact, 50V, 60V and 70V impact is added, the short-circuit indicator lamp is still on and scrapped, the contact electrodes are pressed and short-circuited, the capacitor is discharged, the modulator is reset to zero, and the power switch is switched off;
(16) the electric energizing and impact sieve sheet comprises: the operation process is as follows: inserting a commutator segment between energizing electrodes on the reverse side of an energizing instrument, enabling alloy surfaces to face the same direction, checking whether switches of all parts of the energizing instrument are placed at correct positions, adjusting work according to the room temperature condition, enabling a time-of-rest relay to be normal to guarantee energizing requirements, turning on a main power switch of an energizing table, turning on a starting button switch, continuously working a switch, adjusting energizing voltage, turning on a shunt energizing switch, turning on a shunt short-circuit current adjusting switch to a short-circuit position, immediately adjusting a variable resistor, turning the shunt short-circuit switch to the energizing position, taking off a selenium commutator segment, storing for 24 hours, then carrying out impact test operation, and screening the selenium commutator segments qualified in the impact test;
(17) the reverse measurement is as follows: the operation process is as follows: wearing a rubber finger, taking out the screened qualified selenium sheets, selecting a measuring table according to the sheet type, checking an instrument of the measuring table, switching on a stabilized voltage supply switch and a measuring table switch after the proof of certification is verified, turning on a power supply switch, adjusting the measuring voltage according to a sorting method specified by the measuring table, enabling the alloy surface of the selenium rectifying sheet to face upwards, switching on a test pen for 5 seconds, judging whether the current reading is in a qualified range, switching off the power supply and the stabilized voltage supply after the measurement is finished, switching to the measurement of the measured qualified products, and continuing to electrify the unqualified products;
(18) leading to the measurement: the operation process is as follows: selecting a measuring table according to the sheet shape, wearing a rubber finger, taking out a selenium sheet, switching on a stabilized voltage supply switch and a measuring table switch after checking that the measuring meter is qualified and effective, switching on a test meter pen when the alloy surface of the measuring sheet faces upwards, regulating the current to a rated value, regulating the current, then conducting voltage measurement, switching off the measuring table switch and the stabilized voltage supply switch after measurement, putting the selenium sheet in a specified box according to grouping requirements, and assembling or packaging after the selenium sheet is checked to be qualified;
(19) packaging the finished product, and warehousing for storage: and after the finished product is inspected to be qualified, according to the number of packaged sheets 152-402: every package of 200 pieces, 602-1002: and each package of 50 selenium sheets is firstly wrapped with a layer of damp-proof paper, then wrapped with a layer of kraft paper, printed with selenium sheet specifications, types and red printing oil stamps, and the selenium sheets are individually subjected to blue printing for classification, group, quantity and year, month and day stamps before being delivered to a factory and finally stored in a warehouse.
2. The process of claim 1, wherein the selenium fairing comprises: the selenium preparation and production process comprises the following steps: weighing selenium to be prepared, pouring the selenium into a stainless steel selenium pot, heating and melting the selenium to 300-350 ℃, stirring for 2-8 hours, cooling to 290 ℃, removing scum on the surface of the selenium, adding weighed added selenium, continuously stirring, stirring for 10-40 kg of selenium for 10-20 minutes, calculating the amount of the added selenium according to the weight of the selenium actually produced in the pot, cooling to 240-250 ℃, pouring the selenium into aluminum trays respectively, pouring the selenium which is black, quickly pouring the selenium, avoiding the selenium from falling out at a low temperature, sampling the prepared selenium from the first tray, the middle tray and the last tray respectively, mixing and grinding the selenium into two parts, analyzing the bromine content of the two parts, filling the rest of the selenium into boxes, numbering and placing the boxes on a selenium rack, wherein the bromine content of the selenium is not more than +/-20 percent of the specified amount, and evaporating the selenium is used according to qualified notice.
3. The process of claim 1, wherein the selenium fairing comprises: in the (6) selenium preparation process, the adding weight to be added into the produced selenium is calculated according to the analysis result of bromine content of the added selenium;
calculating the public a ═ B × A/C
a- -weight of selenium required to be added
B- -selenium content required for production
A- - - -the weight of selenium powder filled in the stirring pot
C- -average bromine content in the added selenium.
4. The process of claim 1, wherein the selenium fairing comprises: and (6) determination of bromine in selenium in the selenium preparation process: respectively taking 2-5 g of production selenium and 1-2 g of added selenium analysis samples, putting the analysis samples into a glass mortar, grinding the analysis samples into powder, taking the ground selenium powder by using a ox horn spoon, and putting the powder on a precision balance to weigh 1-5 g; pouring the weighed selenium powder into a cleaned and dried triangular flask with the capacity of 500 ml;
dripping a pre-measured silver nitrate solution of 0.01N into a triangular flask by using an acid dropping pipe to produce 12-15 ml of selenium drops, and adding 20-25 ml of selenium drops; weighing 50ml of silver nitrate by using a measuring cylinder, and pouring into a triangular flask; putting a triangular flask containing silver nitrate and nitric acid samples into a water bath kettle, and heating at a low temperature, wherein the temperature of the water bath kettle is about 100 ℃;
during the selenium dissolving process, a large amount of nitrogen dioxide gas is generated, after the nitrogen dioxide gas is completely volatilized and the selenium is completely dissolved, the triangular flask is immediately taken down, the outer wall is washed by tap water, the temperature is substantially cooled to the room temperature, and water is absolutely prohibited from dripping into the flask; weighing 5ml of toluene, pouring into a triangular flask, weighing 5ml of saturated ammonium ferric alum solution, and pouring into the triangular flask; and measuring 0.01N of ammonium sulfate solution by using an acid burette for titration, wherein in the titration process, the excessive silver nitrate solution in the triangular flask is transparent at first and slightly greenish and then is milky white liquid until the silver nitrate solution is slightly reddish, uniformly shaking the silver nitrate solution until the silver nitrate solution is slightly reddish, and finally recording the data ml of the titrated ammonium thiocyanate.
5. The process of claim 4, wherein the selenium fairing comprises: the solution preparation and calibration in the selenium preparation process in the step (6) are as follows:
in the preparation process, 0.7612gAR ammonium thiocyanate is weighed by a balance and is put into a 1000ml narrow-mouth bottle, distilled water is added to dilute the solution to 1000ml, and the solution is shaken uniformly;
in the calibration, 0.0400g of metal silver is weighed by a precision balance and put into a 300ml triangular flask, then 10ml 1: 1HNO3 is added and shaken firstly to dissolve the silver, then the silver is completely dissolved by heating on an electric furnace, the solution is not overflowed when the heating is carried out, after the nitrogen dioxide gas is volatilized, the heating is stopped, the cooling is carried out, the wall of the flask is washed by distilled water and diluted to about 100ml, after the shaking is even, saturated ferric ammonium alum solution is added, the prepared ammonium thiocyanate is immediately used for titration, and the shaking is carried out while dripping until the prepared ammonium thiocyanate is brick red;
calculating the formula: NH4CN5 concentration-N
N ═ Ag/(NH4CN5 × 0.10788), where the unit of Ag is: g; the measurement units of NH4CN5 are: ml;
the preparation process of the iron ammonium alum solution comprises the following steps:
cleaning and drying a container, weighing according to the solubility of ferric ammonium sulfate, wherein 100g of water is 44.15g at room temperature and 25 ℃, each time is about 500g, then putting the weighed solid ferric ammonium sulfate into distilled water, dissolving to light brown, titrating by using 1: 1 nitric acid until the brown disappears and becomes yellow green, and filtering the solution for use;
the preparation and calibration of the silver nitrate solution are as follows:
during preparation, 1.6989gAR silver nitrate is weighed by a balance, put into a 1000ml narrow-mouth bottle, added with a small amount of distilled water, dissolved, diluted with the distilled water to 1000ml and shaken uniformly;
during calibration, a newly prepared silver nitrate solution with a dropper is poured into a 300ml triangular flask, the solution is diluted by distilled water to about 100ml, 1ml of saturated ferric ammonium alum solution is added, ammonium thiocyanate solution with known concentration is added, the mixture is shaken while being dripped until red appears, and the reading is recorded;
calculating the formula: AgNO3 concentration N
N ═ NH4CNS (ML) × NH4CNS (concentration)/AgNO 3 vol ML was taken out.
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Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2175016A (en) * 1936-06-20 1939-10-03 Gen Electric Method of producing selenium rectifiers or the like
GB522755A (en) * 1937-12-17 1940-06-26 Conradin Kreutzer An improved method of producing selenium rectifiers and selenium photo-cells
US2307474A (en) * 1939-05-26 1943-01-05 Union Switch & Signal Co Manufacture of selenium rectifiers
US2510361A (en) * 1944-04-06 1950-06-06 Hartford Nat Bank & Trust Co Method of producing selenium rectifiers
US2740925A (en) * 1952-02-18 1956-04-03 Int Rectifier Corp Tellurium rectifier and method of making it
US2745047A (en) * 1951-12-14 1956-05-08 Itt Selenium rectifiers and method of manufacture
JPS6234167A (en) * 1985-08-02 1987-02-14 ゼロツクス コ−ポレ−シヨン Light acceptor
CN1752233A (en) * 2005-10-08 2006-03-29 昆明理工大学 Vacuum smelting method for high-thallium coarse cadmium
CN101188199A (en) * 2007-11-20 2008-05-28 中国振华集团永光电子有限公司 A making method for quick recovery silicon rectifying diode chip
CN102031497A (en) * 2009-09-28 2011-04-27 思阳公司 Large scale method and furnace system for selenization of thin film photovoltaic materials
CN103733243A (en) * 2011-08-05 2014-04-16 夏普株式会社 Phosphor substrate, display device, and electronic device
CN105229797A (en) * 2012-10-09 2016-01-06 陶氏环球技术有限责任公司 And have the photovoltaic device of the thin chalcogenide film be electrically interposed between the absorber layers containing pnictide and emitter layer

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2175016A (en) * 1936-06-20 1939-10-03 Gen Electric Method of producing selenium rectifiers or the like
GB522755A (en) * 1937-12-17 1940-06-26 Conradin Kreutzer An improved method of producing selenium rectifiers and selenium photo-cells
US2307474A (en) * 1939-05-26 1943-01-05 Union Switch & Signal Co Manufacture of selenium rectifiers
US2510361A (en) * 1944-04-06 1950-06-06 Hartford Nat Bank & Trust Co Method of producing selenium rectifiers
US2745047A (en) * 1951-12-14 1956-05-08 Itt Selenium rectifiers and method of manufacture
US2740925A (en) * 1952-02-18 1956-04-03 Int Rectifier Corp Tellurium rectifier and method of making it
JPS6234167A (en) * 1985-08-02 1987-02-14 ゼロツクス コ−ポレ−シヨン Light acceptor
CN1752233A (en) * 2005-10-08 2006-03-29 昆明理工大学 Vacuum smelting method for high-thallium coarse cadmium
CN101188199A (en) * 2007-11-20 2008-05-28 中国振华集团永光电子有限公司 A making method for quick recovery silicon rectifying diode chip
CN102031497A (en) * 2009-09-28 2011-04-27 思阳公司 Large scale method and furnace system for selenization of thin film photovoltaic materials
CN103733243A (en) * 2011-08-05 2014-04-16 夏普株式会社 Phosphor substrate, display device, and electronic device
CN105229797A (en) * 2012-10-09 2016-01-06 陶氏环球技术有限责任公司 And have the photovoltaic device of the thin chalcogenide film be electrically interposed between the absorber layers containing pnictide and emitter layer

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《掺铊硒整流片与掺铊硒整流堆》;倪林福 等;《电子技术》;19660630;正文全文 *

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