CN111085827A - Method for manufacturing large-size high-density bright iridium crucible - Google Patents
Method for manufacturing large-size high-density bright iridium crucible Download PDFInfo
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Abstract
The invention provides a method for manufacturing a large-size high-density bright iridium crucible, which comprises the following steps: briquetting and smelting high-purity iridium powder into iridium blocks, putting the iridium blocks into a heat-resistant ceramic crucible and a vacuum intermediate frequency induction furnace for smelting, vacuumizing the vacuum intermediate frequency induction furnace, then filling argon, heating to a complete molten state, slowly condensing iridium liquid, repeating for at least 4 times, and taking out iridium cast ingots; forging into iridium ingots with the thickness of about 20 mm; heating the iridium ingot, then placing the heated iridium ingot on a rolling mill for hot rolling, heating the iridium ingot for once and rolling the iridium ingot for twice, wherein the pressing rates of the two times are reduced in sequence; respectively cutting a crucible bottom and a crucible body from the obtained iridium plate; the working part of the rolling machine is used for rolling the crucible body by the rolling machine made of nickel-based high-temperature alloy; acid washing; welding; trimming, impurity removal and brightening, so that the iridium crucible prepared by the method has the advantages of high density, uniform thickness, bright surface, no bubbling in high-temperature use and long service life.
Description
Technical Field
The invention belongs to the technical field of manufacturing of difficult-to-form noble metals, and particularly relates to a manufacturing method of a large-size high-density bright iridium crucible.
Background
The iridium has a high melting point (2410 + -40 deg.C) and a high density (22.562 + -0.011 g/cm)3) Noble metals with stable chemical properties and good high-temperature oxidation resistance. High-melting-point laser single crystals of Yttrium Aluminum Garnet (YAG), Germanium Gallium Garnet (GGG), wide-bandgap semiconductor gallium nitride, gallium oxide, scintillation crystal (LYSO) and the like are mainly applied to the laser and electronic industries, the demand is very large, the high-melting-point single crystals are generally manufactured by a Czochralski method, and only an iridium crucible can meet the harsh high-temperature production conditions at present, so the practical value and the market prospect of the iridium crucible are self-evident.
The iridium is hard, poor in plasticity and has a transgranular fracture mode at 1000 ℃, so that the iridium belongs to the metal difficult to process. The plasticity of face-centered cubic metals is only exhibited at temperatures above 1200 c, so iridium must be processed at high temperatures.
The traditional casting forming method is that iridium powder or iridium blocks are heated and melted by a medium frequency induction furnace, and iridium melt is directly injected into a magnesium oxide or graphite mold for casting, the production method has a plurality of defects, most of the iridium melt is in contact with air and is easy to absorb air, so that condensed iridium ingots have air holes and small density (less than 19 g/cm)3) And uneven wall thickness, and the like, and can only produce small crucibles with the thickness of less than 50 mm; the traditional plastic forming method has no degassing step, so that air holes exist in the plate, the plate is easy to bubble in high-temperature use, the surface of the plate is rough, the color is grey, and the growth quality of the single crystal is influenced because the surface of the plate is in contact with steel for a long time in the high-temperature processing process and the iron content of the surface is higher.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide a method for manufacturing a large-sized high-density bright iridium crucible, which can solve the problems of low density and uneven wall thickness of an iridium crucible manufactured by a conventional casting method, and the problems of rough surface, coarse crystal grains, gray color, etc. of a conventional plate forming method, and can manufacture an iridium crucible having a high density, uniform wall thickness, and a bright and smooth surface.
The invention provides a method for manufacturing a large-size high-density bright iridium crucible, which is characterized by comprising the following steps of: step 1, preparing high-purity iridium blocks: pressing 99.95% of high-purity iridium powder into blocks by a press machine, and then putting the blocks into a high-vacuum non-consumable arc furnace to be smelted into iridium blocks. After being pressed into blocks by a press machine, the iridium powder with the purity of 99.95 percent is melted into small ingots by a high-vacuum non-consumable electric arc furnace, so that the gas in the powder can be removed, the low-melting-point base metal in the iridium powder is volatilized, and the purity of the iridium is further improved.
Step 2, smelting: putting an iridium block into a heat-resistant ceramic crucible, putting the heat-resistant ceramic crucible into a vacuum medium-frequency induction furnace, vacuumizing the vacuum medium-frequency induction furnace, filling argon into the vacuum medium-frequency induction furnace, heating the iridium block to a completely molten state by the vacuum medium-frequency induction furnace to form iridium liquid, slowly condensing the iridium liquid, rapidly heating and remelting the condensed iridium block, vacuumizing the vacuum medium-frequency induction furnace before remelting, filling argon into the vacuum medium-frequency induction furnace, repeatedly melting and condensing for at least 4 times, and taking out an iridium ingot obtained after condensation. And introducing argon into the high-purity heat-resistant ceramic crucible to prevent the iridium liquid from contacting with air, discharging gas in the condensation process, and before repeatedly melting, re-discharging the gas in the crucible, and then introducing new argon to prevent the iridium block from re-absorbing the previously discharged air in the re-melting process, so that the condensed iridium ingot has no air holes, no cracks and high compactness. The iridium alloy is repeatedly smelted for at least 4 times in the argon environment, so that the gas in the iridium liquid is discharged more thoroughly, the compactness of the iridium cast ingot is greatly improved, and the existence of air holes in the cast ingot is avoided.
The heat-resistant ceramic crucible can be an yttrium-stabilized zirconia crucible, a magnesium-stabilized zirconia crucible, a calcium-stabilized zirconia crucible, or a magnesium oxide crucible.
Step 3, forging: and (3) putting the iridium ingot obtained in the step (2) into a heating furnace, heating to 1400-1600 ℃, preserving heat for 20-60 min, taking out the iridium ingot, forging, putting the iridium ingot into the heating furnace, preserving heat for 5-20 min when the surface temperature of the iridium ingot is lower than 1300 ℃, and repeating the steps until the iridium ingot is forged into an iridium ingot with the thickness of 19-21 mm.
Step 4, hot rolling: and (3) putting the iridium ingot obtained by forging in the step (3) into a vacuum furnace, heating to 1300-1500 ℃, preserving heat for 15-40 min, taking out the iridium ingot, rolling twice on a rolling mill, wherein the pressing rates of the two times are 10-15% and 4-8% in sequence, then putting into a furnace, preserving heat for 5-20 min, and repeating the steps until the iridium plate is rolled to the thickness of the crucible to be prepared. The dynamic recrystallization in the rolling process is ensured by two times of rolling once by heating, thereby not only ensuring the yield of the iridium plate, but also shortening the whole working hour. And in the two-time rolling, the pressing rate is gradually reduced, so that the cracks generated in the iridium plate rolling process can be greatly reduced. Specifically, the rolling mill employs a two-high reversing hot rolling mill of the general type. Optimally, the iridium plate is rolled in proportion, so that the rolled iridium plate is more uniform, and the wall thickness difference between the thinnest part and the thickest part is 0.02 mm.
Step 5, wire cutting: and (4) respectively cutting the iridium plate obtained in the step (4) into a crucible bottom and a crucible body plate with the required sizes by adopting linear cutting.
Step 6, hot curling and forming: and (3) heating the crucible body plate cut out in the step (5) to 1000-1300 ℃, and then rolling by using a rolling machine, wherein the working part of the rolling machine is made of nickel-based high-temperature alloy, the rolling is performed isothermally during rolling, and the alignment and tightness of the interface are ensured during rolling and forming. The working part of the rolling machine is made of nickel-based high-temperature alloy so as to prevent the surface of the iridium plate from being stained with iron elements. The iridium plate has good plasticity in the whole rolling process by isothermal rolling during rolling, and an iridium crucible body with aligned and compact interfaces is obtained during rolling forming.
And 7, acid washing, namely putting the crucible body prepared in the step 6 into hydrochloric acid solution with the concentration of 20-38%, boiling the acid solution, and then preserving the heat for 10-40 min.
Step 8, welding: and (3) under the protection of argon, welding the crucible bottom cut out in the step (5) and the crucible body pickled in the step (7) by using plasma arc welding, and using iridium wire as a welding flux to prepare the iridium crucible.
Step 9, trimming, impurity removal and brightening: and (4) trimming, impurity removing and brightening the iridium crucible prepared in the step (8) in sequence.
Further, in the method for manufacturing the large-size high-density bright iridium crucible provided by the invention, the method can also have the following characteristics: the specific method for preparing the high-purity iridium block in the step 1 comprises the following steps: putting iridium powder with the purity of more than 99.95% into an alloy steel briquetting mould, putting the alloy steel briquetting mould into a 500T-800T hydraulic press, maintaining the pressure for 20s-25s to obtain wafers with the diameter of 30mm-50mm and the thickness of 20mm-30mm, respectively putting the wafers into each water-cooled copper crucible of a vacuum non-consumable electric arc furnace, operating the water-cooled copper-tungsten electrodes to carry out electric arc melting on the wafers, and when in melting, ensuring that the vacuum degree in the vacuum non-consumable electric arc furnace is less than or equal to 3 multiplied by 10-3Pa, keeping for 10-20 s after all the materials are melted, closing the electric arc, and cooling the iridium liquid in a water-cooled copper crucible to obtain an iridium block.
Further, in the method for manufacturing the large-size high-density bright iridium crucible provided by the invention, the method can also have the following characteristics: and 2, putting the heat-resistant ceramic crucible containing the iridium blocks into a vacuum medium-frequency induction furnace, putting a water-cooled copper mold together, heating the condensed iridium blocks to 2550-2600 ℃ for complete melting during the last melting and condensation, then preserving the heat at 2450-2500 ℃ for 1-3 min, then casting into the water-cooled copper mold, and cooling to form iridium cast ingots.
Further, in the method for manufacturing the large-size high-density bright iridium crucible provided by the invention, the method can also have the following characteristics: in step 2, the number of times of melting and condensing is 4.
Further, in the method for manufacturing the large-size high-density bright iridium crucible provided by the invention, the method can also have the following characteristics: in step 2, vacuumizing the vacuum intermediate frequency induction furnace to ensure that the vacuum degree in the vacuum intermediate frequency induction furnace is less than or equal to 5 multiplied by 10-2Pa, and then filling argon into the vacuum intermediate frequency induction furnace to ensure that the pressure in the vacuum intermediate frequency induction furnace is 400-1000 Pa.
Further, in the method for manufacturing the large-size high-density bright iridium crucible provided by the invention, the method can also have the following characteristics: in the step 2, after the iridium liquid is slowly condensed into iridium blocks, the temperature of the iridium blocks is lower than the melting point of iridium and is not more than 10 ℃. This saves remelting time. During specific operation, the power of the vacuum intermediate frequency induction furnace is adjusted, so that the condensation of the iridium liquid is not excessive.
Further, in the method for manufacturing the large-size high-density bright iridium crucible provided by the invention, the method can also have the following characteristics: before the iridium ingot obtained in the step 2 is placed into a heating furnace for heating, the iridium ingot obtained in the step 2 is soaked in dilute nitric acid at the temperature of 50-90 ℃, then is dried, after the iridium ingot with the required thickness is obtained, the iridium ingot is placed into the heating furnace for heat preservation for 5-20 min, and then is placed into clear water for quenching, so that a bright iridium ingot is obtained.
Further, in the method for manufacturing the large-size high-density bright iridium crucible provided by the invention, the method can also have the following characteristics: before the iridium ingot forged in the step 3 is placed in a heating furnace to be heated, the iridium ingot forged in the step 3 is soaked in concentrated hydrochloric acid at the temperature of 50-90 ℃, then is dried, after an iridium plate with the required thickness is obtained, the iridium plate is placed in the heating furnace to be kept for 5-20 min, and then is placed in clear water to be quenched, so that a bright iridium plate is obtained.
Further, in the method for manufacturing the large-size high-density bright iridium crucible provided by the invention, the method can also have the following characteristics: wherein in the step 6, before the crucible body plate prepared in the step 5 is heated, the crucible body plate prepared in the step 5 is firstly soaked in concentrated hydrochloric acid at the temperature of 50-90 ℃ and then dried,
the specific operation method of isothermal edge rolling comprises the following steps: and continuously carrying out temperature compensation heating on the iridium plate by using oxyhydrogen flame in the rounding process so as to keep the temperature of the plate of the crucible body unchanged.
Further, in the method for manufacturing the large-size high-density bright iridium crucible provided by the invention, the method can also have the following characteristics: wherein, in the step 8, the purity of the iridium wire used as the solder is more than 99.95 percent. After the welding is finished, the temperature of the part to be welded is reduced to be below 500 ℃, and then the argon gas is removed.
Further, in the method for manufacturing the large-size high-density bright iridium crucible provided by the invention, the method can also have the following characteristics: in the step 9, the specific operation method of trimming, impurity removal and brightening comprises the following steps: cutting the opening of the iridium crucible prepared in the step 8 into a uniform shape by wire cut electrical discharge, immersing the iridium crucible into a concentrated sodium hydroxide solution at the temperature of 50-90 ℃, placing the concentrated sodium hydroxide solution into a heatable ultrasonic cleaning machine, carrying out ultrasonic treatment for 10-30 min, removing impurities possibly stained on the surface, then placing the iridium crucible into a vacuum annealing furnace, carrying out heat preservation for 10-30 min at the temperature of 1150-1300 ℃, annealing along with the furnace, then placing the iridium crucible into a magnetic polishing machine for treatment, then placing the iridium crucible into a hydrochloric acid solution with the concentration of 20-38% for heating to boiling, carrying out heat preservation for 10-40 min, cleaning, drying, and packaging and storing by a preservative film.
The invention has the following advantages:
the manufacturing method of the large-size high-density bright iridium crucible related by the invention comprises the steps of briquetting and smelting high-purity iridium powder into an iridium block, repeatedly smelting the iridium block for more than 4 times in an argon environment, forging an iridium cast ingot, heating the iridium ingot, then placing the iridium ingot on a rolling mill for hot rolling, heating for once and rolling for twice, and sequentially reducing the pressing rate of twice; and then performing wire cutting, isothermal rolling, acid washing, welding, trimming, impurity removal, brightening and other treatments to prepare the iridium crucible.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the manufacturing method of the large-size high-density bright iridium crucible of the invention is specifically described below with reference to the embodiments.
Example one
Manufacturing an iridium crucible with a diameter of 60 mm:
step 1, preparing high-purity iridium blocks, pressing 99.95% of high-purity iridium powder into blocks by using a press machine, and thenThen putting the iridium block into a high-vacuum non-consumable electric arc furnace to be smelted into an iridium block. The specific method comprises the following steps: putting iridium powder with the purity of more than 99.95% into an alloy steel briquetting mould, putting the alloy steel briquetting mould into a 500T hydraulic press, maintaining the pressure for 25s to obtain wafers with the diameter of 30mm and the thickness of 20mm, repeating the process to obtain a certain amount of wafers, respectively putting the prepared wafers into each water-cooled copper crucible of a vacuum non-consumable arc furnace, operating the water-cooled copper tungsten electrodes to carry out arc melting on the wafers, wherein the vacuum degree in the vacuum non-consumable arc furnace is 3 multiplied by 10 during melting-3Pa, keeping for 20s after all the materials are melted, closing the electric arc, and cooling the iridium liquid in a water-cooled copper crucible to obtain an iridium block.
Step 2, smelting: putting the iridium block obtained in the step 1 into an yttrium stabilized zirconia crucible, putting the yttrium stabilized zirconia crucible filled with the iridium block and a water-cooled copper mold into a vacuum medium-frequency induction furnace, and vacuumizing the vacuum medium-frequency induction furnace to ensure that the vacuum degree in the vacuum medium-frequency induction furnace is 5 multiplied by 10-2Pa, filling argon into the vacuum intermediate frequency induction furnace to ensure that the pressure in the vacuum intermediate frequency induction furnace is 400Pa, heating the iridium block to a completely molten state by the vacuum intermediate frequency induction furnace to form iridium liquid, slowly condensing the iridium liquid, ensuring that the temperature of the condensed iridium block is lower than the melting point of iridium and does not exceed 10 ℃ by adjusting the power of the vacuum intermediate frequency induction furnace, quickly heating and remelting the condensed iridium block, vacuumizing the vacuum intermediate frequency induction furnace before remelting to ensure that the vacuum degree in the vacuum intermediate frequency induction furnace is 5 multiplied by 10-2Pa, then filling argon to ensure that the pressure in the vacuum intermediate frequency induction furnace is 400Pa, repeating melting and condensing for 4 times, heating the condensed iridium block to 2550 ℃ for complete melting during melting and condensing for the fourth time, then reducing the power of the vacuum intermediate frequency induction furnace, preserving the heat at 2450 ℃ for 3min, then casting into a water-cooled copper mold, and cooling to form an iridium ingot.
Step 3, forging: soaking the iridium ingot obtained in the step 2 in dilute nitric acid at 50 ℃ and then drying the iridium ingot, then placing the iridium ingot into a silicon-molybdenum rod heating furnace to heat to 1400 ℃, preserving heat for 40min, then taking out the iridium ingot to forge, monitoring the surface temperature of the iridium ingot in real time by using an infrared thermometer, placing the iridium ingot into the heating furnace to preserve heat for 5min when the surface temperature of the iridium ingot is lower than 1300 ℃, repeating the steps until the iridium ingot is forged into an iridium ingot with the thickness of 19mm-21mm, then placing the iridium ingot into the heating furnace to preserve heat for 5min, and then placing the iridium ingot into clear water to quench so as to obtain a bright iridium ingot.
Step 4, hot rolling: and (3) soaking the iridium ingot forged in the step (3) with concentrated hydrochloric acid at 50 ℃, drying the iridium ingot, then placing the iridium ingot into a vacuum furnace, heating the iridium ingot to 1300 ℃, preserving heat for 15min, then taking out the iridium ingot, rolling the iridium ingot on a rolling mill twice, keeping the pressing rate of the iridium ingot twice at 15% and 8% in sequence, then placing the iridium ingot into the furnace, preserving heat for 5min, and repeating the steps until the iridium plate is rolled to the thickness of the crucible to be prepared. And then putting the iridium plate into a heating furnace, preserving the heat for 5min, and then putting the iridium plate into clear water for quenching to obtain a bright iridium plate. The detection shows that the wall thickness difference between the thinnest part and the thickest part of the iridium plate is 0.02 mm. In the present embodiment, the proportional rolling is adopted in the iridium rolling.
Step 5, wire cutting: and (4) respectively cutting the iridium plate obtained in the step (4) into a crucible bottom and a crucible body plate with the required sizes by adopting linear cutting. Specifically, the iridium plate obtained in step 4 is cut by wire electrical discharge machining, and the iridium in the coolant is recovered after the cutting is completed. The electric spark wire cutting is adopted for blanking, the size precision of the plate is within 0.01mm, the notch is straight, and the subsequent rolling welding is easy.
Step 6, hot curling and forming: and (3) soaking the crucible body plate cut out in the step (5) with concentrated hydrochloric acid at 50 ℃ and then drying the crucible body plate, heating the crucible body plate to 1000 ℃, rolling the crucible body plate by using a rolling machine, wherein the working part of the rolling machine is made of nickel-based high-temperature alloy, and continuously performing temperature supplementing heating on the iridium plate by using oxyhydrogen flame in the rolling process to keep the temperature of the crucible body plate at 1000 ℃, so that the alignment and tightness of the interfaces are ensured during the rolling and forming.
And 7, acid washing, namely putting the crucible body prepared in the step 6 into a hydrochloric acid solution with the concentration of 20%, boiling the acid solution, and then preserving the heat for 40 min.
Step 8, welding: and (3) under the protection of argon, welding the crucible bottom cut out in the step (5) and the crucible body pickled in the step (7) by plasma arc welding, taking iridium wires with the purity of more than 99.95% as welding flux, cooling the temperature of the part to be welded to be below 500 ℃ after the welding is finished, and removing the argon to obtain the iridium crucible with bright welding line and 60mm diameter.
Step 9, trimming, impurity removal and brightening: trimming, impurity removal and brightness treatment: and (4) trimming, impurity removing and brightening the iridium crucible prepared in the step (8) in sequence. The specific operation method of trimming, impurity removing and brightening treatment comprises the following steps: cutting the opening of the iridium crucible prepared in the step 8 into a uniform shape by wire electrical discharge cutting, then immersing the iridium crucible into a concentrated sodium hydroxide solution at 50 ℃, placing the concentrated sodium hydroxide solution into a heatable ultrasonic cleaning machine, carrying out ultrasonic treatment for 30min, removing impurities possibly stained on the surface, then placing the iridium crucible into a vacuum annealing furnace, carrying out heat preservation for 30min at 1150 ℃, annealing along with the furnace, then placing the iridium crucible into a magnetic polishing machine for treatment, then placing the iridium crucible into a hydrochloric acid solution with the concentration of 20%, heating to boiling, carrying out heat preservation for 40min, cleaning, drying, and then packaging and storing by using a preservative film.
The prepared iridium crucible has bright and smooth surface and uniform thickness, and the detected density of the iridium crucible is 22.556g/cm3Iron content<30ppm。
Example two
Manufacturing an iridium crucible with a diameter of 150 mm:
step 1, preparing a high-purity iridium block, pressing more than 99.95% of high-purity iridium powder into a block by using a press machine, and then putting the block into a high-vacuum non-consumable electric arc furnace to be melted into the iridium block. The specific method comprises the following steps: putting iridium powder with the purity of more than 99.95% into an alloy steel briquetting mould, putting the alloy steel briquetting mould into a 600T hydraulic press, maintaining the pressure for 23s to obtain wafers with the diameter of 40mm and the thickness of 30mm, repeating the process to obtain a certain amount of wafers, respectively putting the prepared wafers into each water-cooled copper crucible of a vacuum non-consumable arc furnace, operating the water-cooled copper tungsten electrodes to carry out arc melting on the wafers, wherein the vacuum degree in the vacuum non-consumable arc furnace is 2 multiplied by 10 during melting-3Pa, keeping for 10s after all the materials are melted, closing the electric arc, and cooling the iridium liquid in a water-cooled copper crucible to obtain an iridium block.
Step 2, smelting: putting the iridium blocks obtained in the step 1 into a magnesium-stabilized zirconia crucible, and adding magnesium-stabilized oxygen filled with the iridium blocksThe zirconium crucible and the water-cooled copper mold are arranged in a vacuum intermediate frequency induction furnace, and then the vacuum medium frequency induction furnace is vacuumized, so that the vacuum degree in the vacuum intermediate frequency induction furnace is 6 multiplied by 10-3Pa, filling argon into the vacuum intermediate frequency induction furnace to ensure that the pressure in the vacuum intermediate frequency induction furnace is 1000Pa, heating the iridium block to a completely molten state by the vacuum intermediate frequency induction furnace to form iridium liquid, slowly condensing the iridium liquid, ensuring that the temperature of the condensed iridium block is lower than the melting point of iridium and does not exceed 10 ℃ by adjusting the power of the vacuum intermediate frequency induction furnace, quickly heating and remelting the condensed iridium block, vacuumizing the vacuum intermediate frequency induction furnace before remelting to ensure that the vacuum degree in the vacuum intermediate frequency induction furnace is 6 multiplied by 10-3Pa, then filling argon to ensure that the pressure in the vacuum intermediate frequency induction furnace is 1000Pa, repeating melting and condensing for 4 times, heating the condensed iridium block to 2600 ℃ for complete melting during melting and condensing for the fourth time, then reducing the power of the vacuum intermediate frequency induction furnace, preserving the heat at 2500 ℃ for 1min, then casting into a water-cooled copper mold, and cooling to form an iridium ingot.
Step 3, forging: soaking the iridium ingot obtained in the step 2 in dilute nitric acid at 90 ℃, drying the iridium ingot, then placing the iridium ingot into a silicon-molybdenum rod heating furnace, heating the iridium ingot to 1600 ℃, preserving heat for 20min, then taking out the iridium ingot, forging the iridium ingot, monitoring the surface temperature of the iridium ingot in real time by using an infrared thermometer, placing the iridium ingot into the heating furnace for preserving heat for 20min when the surface temperature of the iridium ingot is lower than 1300 ℃, repeating the steps until the iridium ingot is forged into an iridium ingot with the thickness of 19mm-21mm, then placing the iridium ingot into the heating furnace for preserving heat for 10min, and then placing the iridium ingot into clear water for quenching to obtain a bright iridium ingot.
Step 4, hot rolling: and (3) soaking the iridium ingot forged in the step (3) with concentrated hydrochloric acid at 70 ℃, drying the iridium ingot, then placing the iridium ingot into a vacuum furnace, heating the iridium ingot to 1500 ℃, preserving heat for 30min, then taking out the iridium ingot, rolling the iridium ingot on a rolling mill twice, keeping the pressing rate of the iridium ingot twice at 10% and 4% in sequence, then placing the iridium ingot into the furnace, preserving heat for 15min, and repeating the steps until the iridium plate is rolled to the thickness of the crucible to be prepared. And then putting the iridium plate into a heating furnace, preserving the heat for 20min, and then putting the iridium plate into clear water for quenching to obtain a bright iridium plate. The detection shows that the wall thickness difference between the thinnest part and the thickest part of the iridium plate is 0.01 mm. In the present embodiment, the proportional rolling is adopted in the iridium rolling.
Step 5, wire cutting: and (4) respectively cutting the iridium plate obtained in the step (4) into a crucible bottom and a crucible body plate with the required sizes by adopting linear cutting. Specifically, the iridium plate obtained in step 4 is cut by wire electrical discharge machining, and the iridium in the coolant is recovered after the cutting is completed. The electric spark wire cutting is adopted for blanking, the size precision of the plate is within 0.01mm, the notch is straight, and the subsequent rolling welding is easy.
Step 6, hot curling and forming: and (3) soaking the crucible body plate cut out in the step (5) with concentrated hydrochloric acid at 90 ℃, drying the crucible body plate, heating the crucible body plate to 1200 ℃, rolling the crucible body plate by using a rolling machine, wherein the working part of the rolling machine is made of nickel-based high-temperature alloy, and continuously performing temperature supplementing heating on the iridium plate by using oxyhydrogen flame in the rolling process to keep the temperature of the crucible body plate at 1200 ℃, so that the interfaces are aligned and compact during rolling and forming.
And 7, acid washing, namely putting the crucible body prepared in the step 6 into a hydrochloric acid solution with the concentration of 30%, boiling the acid solution, and then preserving the heat for 20 min.
Step 8, welding: and (3) under the protection of argon, welding the crucible bottom cut out in the step (5) and the crucible body pickled in the step (7) by plasma arc welding, taking iridium wires with the purity of more than 99.95% as welding flux, cooling the temperature of the part to be welded to be below 500 ℃ after the welding is finished, and removing the argon to obtain the iridium crucible with bright welding line and 150mm diameter.
Step 9, trimming, impurity removal and brightening: trimming, impurity removal and brightness treatment: and (4) trimming, impurity removing and brightening the iridium crucible prepared in the step (8) in sequence. The specific operation method of trimming, impurity removing and brightening treatment comprises the following steps: cutting the opening of the iridium crucible prepared in the step 8 into a uniform shape by wire electrical discharge cutting, immersing the iridium crucible into a concentrated sodium hydroxide solution at 90 ℃, placing the concentrated sodium hydroxide solution into a heatable ultrasonic cleaning machine, carrying out ultrasonic treatment for 15min, removing impurities possibly stained on the surface, then placing the iridium crucible into a vacuum annealing furnace, carrying out heat preservation for 15min at 1200 ℃, annealing along with the furnace, then placing the iridium crucible into a magnetic polishing machine for treatment, then placing the iridium crucible into a hydrochloric acid solution with the concentration of 30%, heating to boiling, carrying out heat preservation for 30min, cleaning, drying, and packaging and storing by a preservative film.
The prepared iridium crucible has bright and smooth surface and uniform thickness, and the detected density of the iridium crucible is 22.561g/cm3Iron content<30ppm。
EXAMPLE III
Manufacturing an iridium crucible with a diameter of 300 mm:
step 1, preparing a high-purity iridium block, pressing more than 99.95% of high-purity iridium powder into a block by using a press machine, and then putting the block into a high-vacuum non-consumable electric arc furnace to be melted into the iridium block. The specific method comprises the following steps: putting iridium powder with the purity of more than 99.95% into an alloy steel briquetting mould, putting the alloy steel briquetting mould into a 800T hydraulic press, maintaining the pressure for 20s to obtain wafers with the diameter of 50mm and the thickness of 25mm, repeating the process to obtain a certain amount of wafers, respectively putting the prepared wafers into each water-cooled copper crucible of a vacuum non-consumable arc furnace, operating the water-cooled copper tungsten electrodes to carry out arc melting on the wafers, wherein the vacuum degree in the vacuum non-consumable arc furnace is 2 multiplied by 10 during melting-3Pa, keeping for 15s after all the materials are melted, closing the electric arc, and cooling the iridium liquid in a water-cooled copper crucible to obtain an iridium block.
Step 2, smelting: putting the iridium blocks obtained in the step 1 into a magnesium oxide crucible, putting the magnesium oxide crucible filled with the iridium blocks and a water-cooled copper mold into a vacuum medium-frequency induction furnace, and vacuumizing the vacuum medium-frequency induction furnace to ensure that the vacuum degree in the vacuum medium-frequency induction furnace is less than or equal to 5 multiplied by 10-2Pa, filling argon into the vacuum intermediate frequency induction furnace to ensure that the pressure in the vacuum intermediate frequency induction furnace is 400-1000 Pa, heating the iridium block to a completely molten state by the vacuum intermediate frequency induction furnace to form iridium liquid, slowly condensing the iridium liquid, regulating the power of the vacuum intermediate frequency induction furnace to ensure that the temperature of the condensed iridium block is lower than the melting point of iridium and does not exceed 10 ℃, quickly heating and remelting the condensed iridium block, vacuumizing the vacuum intermediate frequency induction furnace before remelting to ensure that the vacuum degree in the vacuum intermediate frequency induction furnace is less than or equal to 5 multiplied by 10-2Pa, then filling argon to ensure that the pressure in the vacuum intermediate frequency induction furnace is 400Pa-1000Pa and the weight is heavyAnd melting and condensing for 5 times, heating the condensed iridium blocks to 2555 ℃ for complete melting during melting and condensing for the fifth time, then reducing the power of the vacuum intermediate frequency induction furnace, preserving heat at 2455 ℃ for 2min, then casting into a water-cooled copper mold, and cooling to form iridium ingots. In this embodiment, when 5 times of melting and condensing are performed, the degree of vacuum in the vacuum intermediate frequency induction furnace is less than or equal to 5 × 10-2Pa is not needed to be the same each time, and the pressure of argon filled in the vacuum intermediate frequency induction furnace is 400Pa-1000Pa, and the pressure does not need to be the same each time.
Step 3, forging: soaking the iridium ingot obtained in the step 2 in dilute nitric acid at 70 ℃, drying the iridium ingot, then placing the iridium ingot in a silicon-molybdenum rod heating furnace, heating to 1500 ℃, preserving heat for 60min, then taking out the iridium ingot, forging, monitoring the surface temperature of the iridium ingot in real time by using an infrared thermometer, placing the iridium ingot in the heating furnace for preserving heat for 15min when the surface temperature of the iridium ingot is lower than 1300 ℃, repeating the steps until the iridium ingot is forged into an iridium ingot with the thickness of 19mm-21mm, then placing the iridium ingot in the heating furnace for preserving heat for 20min, and then placing the iridium ingot in clean water for quenching to obtain a bright iridium ingot.
Step 4, hot rolling: and (3) soaking the iridium ingot forged in the step (3) with concentrated hydrochloric acid at 90 ℃, drying the iridium ingot, then placing the iridium ingot into a vacuum furnace, heating the iridium ingot to 1400 ℃, preserving heat for 40min, then taking out the iridium ingot, rolling the iridium ingot on a rolling mill twice, keeping the pressing rate of the iridium ingot twice at 12% and 6% in sequence, then placing the iridium ingot into the furnace, preserving heat for 20min, and repeating the steps until the iridium plate is rolled to the thickness of the crucible to be prepared. And then putting the iridium plate into a heating furnace, preserving the heat for 15min, and then putting the iridium plate into clear water for quenching to obtain a bright iridium plate. The detection shows that the wall thickness difference between the thinnest part and the thickest part of the iridium plate is 0.02 mm. In the present embodiment, the proportional rolling is adopted in the iridium rolling.
Step 5, wire cutting: and (4) respectively cutting the iridium plate obtained in the step (4) into a crucible bottom and a crucible body plate with the required sizes by adopting linear cutting. Specifically, the iridium plate obtained in step 4 is cut by wire electrical discharge machining, and the iridium in the coolant is recovered after the cutting is completed. The electric spark wire cutting is adopted for blanking, the size precision of the plate is within 0.01mm, the notch is straight, and the subsequent rolling welding is easy.
Step 6, hot curling and forming: and (3) soaking the crucible body plate cut out in the step (5) with concentrated hydrochloric acid at 60 ℃, drying the crucible body plate, heating the crucible body plate to 1300 ℃, rolling the crucible body plate by using a rolling machine, wherein the working part of the rolling machine is made of nickel-based high-temperature alloy, and continuously performing temperature supplementing heating on the iridium plate by using oxyhydrogen flame in the rolling process to keep the temperature of the crucible body plate at 1300 ℃, so that the interfaces are aligned and compact during rolling and forming.
And 7, acid washing, namely putting the crucible body prepared in the step 6 into a hydrochloric acid solution with the concentration of 38%, boiling the acid solution, and then preserving the heat for 10 min.
Step 8, welding: and (3) under the protection of argon, welding the crucible bottom cut out in the step (5) and the crucible body pickled in the step (7) by plasma arc welding, taking iridium wires with the purity of more than 99.95% as welding flux, cooling the temperature of the part to be welded to be below 500 ℃ after the welding is finished, and removing the argon to obtain the iridium crucible with bright welding line and the diameter of 300 mm.
Step 9, trimming, impurity removal and brightening: trimming, impurity removal and brightness treatment: and (4) trimming, impurity removing and brightening the iridium crucible prepared in the step (8) in sequence. The specific operation method of trimming, impurity removing and brightening treatment comprises the following steps: cutting the opening of the iridium crucible prepared in the step 8 into a uniform shape by wire electrical discharge cutting, immersing the iridium crucible into a concentrated sodium hydroxide solution at the temperature of 80 ℃, placing the concentrated sodium hydroxide solution into a heatable ultrasonic cleaning machine, carrying out ultrasonic treatment for 10min, removing impurities possibly stained on the surface, then placing the iridium crucible into a vacuum annealing furnace, carrying out heat preservation for 10min at the temperature of 1300 ℃, annealing along with the furnace, then placing the iridium crucible into a magnetic polishing machine for treatment, then placing the iridium crucible into a hydrochloric acid solution with the concentration of 38%, heating to boiling, carrying out heat preservation for 10min, cleaning, drying, and then packaging and storing by using a preservative film.
The prepared iridium crucible has bright and smooth surface and uniform thickness, and the detected density of the iridium crucible is 22.553g/cm3Iron content<30ppm。
The iridium crucible prepared in the three embodiments does not generate a bubbling phenomenon in a high-temperature long-term use process, and the service life of the iridium crucible reaches more than 3000 hours at the temperature of 2100 ℃.
The method obtains the high-density bright iridium crucible through the processes of vacuum arc melting degassing, hot rolling recrystallization, isothermal edge rolling, wire cutting, plasma welding under atmosphere protection, vacuum annealing, magnetic polishing and the like, and solves the problems of small density, uneven wall thickness, rough surface, coarse grains, gray color and the like of the conventional plate forming method of the iridium crucible in the conventional casting method.
The iridium crucible manufactured by the method has large size range (the crucible with the diameter of 50mm-300mm can be manufactured), uniform thickness (the wall thickness difference between the thinnest part and the thickest part is less than or equal to 0.02mm), bright and smooth surface and large density (more than or equal to 22.55 g/cm)3) The iridium crucible has high integral purity and iron content<30ppm, no bubbling phenomenon can occur in the high-temperature long-term use process, and the service life can reach more than 3000 hours at the temperature of 2100 ℃.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.
Claims (10)
1. The manufacturing method of the large-size high-density bright iridium crucible is characterized by comprising the following steps of:
step 1, preparing high-purity iridium blocks: pressing 99.95% of high-purity iridium powder into blocks by using a press machine, and then putting the blocks into a high-vacuum non-consumable electric arc furnace to be smelted into iridium blocks;
step 2, smelting: putting an iridium block into a heat-resistant ceramic crucible, putting the heat-resistant ceramic crucible into a vacuum medium-frequency induction furnace, vacuumizing the vacuum medium-frequency induction furnace, filling argon into the vacuum medium-frequency induction furnace, heating the iridium block to a completely molten state by the vacuum medium-frequency induction furnace to form iridium liquid, slowly condensing the iridium liquid, rapidly heating and remelting the condensed iridium block, vacuumizing the vacuum medium-frequency induction furnace before remelting, filling argon into the vacuum medium-frequency induction furnace, repeatedly melting and condensing for at least 4 times, and taking out an iridium cast ingot obtained after condensation;
step 3, forging: putting the iridium ingot obtained in the step 2 into a heating furnace, heating to 1400-1600 ℃, preserving heat for 20-60 min, then taking out the iridium ingot, forging, putting the iridium ingot into the heating furnace, preserving heat for 5-20 min when the surface temperature of the iridium ingot is lower than 1300 ℃, and repeating the steps until the iridium ingot is forged into an iridium ingot with the thickness of 19-21 mm;
step 4, hot rolling: putting the iridium ingot obtained by forging in the step 3 into a vacuum furnace, heating to 1300-1500 ℃, preserving heat for 15-40 min, taking out the iridium ingot, rolling twice on a rolling mill, wherein the pressing rates of the two times are 10-15% and 4-8% in sequence, then putting the iridium ingot into the furnace, preserving heat for 5-20 min, and repeating the steps until the iridium plate is rolled to the thickness of the crucible to be prepared;
step 5, wire cutting: respectively cutting the iridium plate obtained in the step 4 into a crucible bottom and a crucible body plate with the prepared size by adopting linear cutting;
step 6, hot curling and forming: heating the crucible body plate cut out in the step 5 to 1000-1300 ℃, and then rolling by using a rolling machine, wherein the working part of the rolling machine is made of nickel-based high-temperature alloy, the rolling is performed isothermally during rolling, and the interfaces are ensured to be aligned and compact during rolling forming;
step 7, acid washing, namely placing the crucible body prepared in the step 6 into hydrochloric acid solution with the concentration of 20% -38%, boiling the acid solution, and then preserving the heat for 10min-40 min;
step 8, welding: under the protection of argon, welding the crucible bottom cut out in the step 5 and the crucible body pickled in the step 7 by plasma arc welding, and taking iridium wires as welding flux to prepare the iridium crucible;
step 9, trimming, impurity removal and brightening: and (4) trimming, impurity removing and brightening the iridium crucible prepared in the step (8) in sequence.
2. The method of manufacturing a large size high density bright iridium crucible as recited in claim 1, wherein:
the specific method for preparing the high-purity iridium block in the step 1 comprises the following steps: putting iridium powder with the purity of more than 99.95% into an alloy steel briquetting mould, putting the alloy steel briquetting mould into a 500T-800T hydraulic press, maintaining the pressure for 20s-25s to obtain wafers with the diameter of 30mm-50mm and the thickness of 20mm-30mm, respectively putting the wafers into each water-cooled copper crucible of a vacuum non-consumable electric arc furnace, and operating waterArc melting the wafer with cold copper-tungsten electrode under vacuum degree of 3 × 10-3Pa, keeping for 10-20 s after all the materials are melted, closing the electric arc, and cooling the iridium liquid in a water-cooled copper crucible to obtain an iridium block.
3. The method of manufacturing a large size high density bright iridium crucible as recited in claim 1, wherein:
and 2, putting the heat-resistant ceramic crucible filled with the iridium blocks into a vacuum medium-frequency induction furnace, putting a water-cooled copper mold together, heating the condensed iridium blocks to 2550-2600 ℃ for complete melting during the last melting and condensation, then preserving the heat at 2450-2500 ℃ for 1-3 min, then casting into the water-cooled copper mold, and cooling to form iridium ingots.
4. The method of manufacturing a large size high density bright iridium crucible as recited in claim 1, wherein:
in step 2, the number of times of melting and condensing is 4.
5. The method of manufacturing a large size high density bright iridium crucible as recited in claim 1, wherein:
in step 2, vacuumizing the vacuum intermediate frequency induction furnace to ensure that the vacuum degree in the vacuum intermediate frequency induction furnace is less than or equal to 5 multiplied by 10-2Pa, and then filling argon into the vacuum intermediate frequency induction furnace to ensure that the pressure in the vacuum intermediate frequency induction furnace is 400-1000 Pa.
6. The method of manufacturing a large size high density bright iridium crucible as recited in claim 1, wherein:
in step 3, before the iridium cast ingot obtained in the step 2 is placed into a heating furnace for heating, the iridium cast ingot obtained in the step 2 is soaked in dilute nitric acid at the temperature of 50-90 ℃ and then dried,
and after obtaining the iridium ingot with the required thickness, putting the iridium ingot into a heating furnace, preserving the heat for 5-20 min, and then putting the iridium ingot into clear water for quenching to obtain a bright iridium ingot.
7. The method of manufacturing a large size high density bright iridium crucible as recited in claim 1, wherein:
in step 4, before the iridium ingot forged in the step 3 is put into a heating furnace for heating, the iridium ingot forged in the step 3 is soaked in concentrated hydrochloric acid at 50-90 ℃ and then dried,
after the iridium plate with the required thickness is obtained, the iridium plate is placed into a heating furnace to be insulated for 5min-20min, and then the iridium plate is placed into clear water to be quenched, so that the bright iridium plate is obtained.
8. The method of manufacturing a large size high density bright iridium crucible as recited in claim 1, wherein:
in step 6, before heating the crucible body plate prepared in step 5, the crucible body plate prepared in step 5 is soaked in concentrated hydrochloric acid at 50-90 ℃ and then dried,
the specific operation method of isothermal edge rolling comprises the following steps: and continuously carrying out temperature supplementing heating on the iridium plate by using oxyhydrogen flame in the rounding process so as to keep the temperature unchanged.
9. The method of manufacturing a large size high density bright iridium crucible as recited in claim 1, wherein:
in step 8, after the welding is finished, the temperature of the part to be welded is reduced to be below 500 ℃, and then argon is removed.
10. The method of manufacturing a large size high density bright iridium crucible as recited in claim 1, wherein:
in step 9, the specific operation method of trimming, impurity removal and brightening treatment comprises the following steps: cutting the opening of the iridium crucible prepared in the step 8 into a whole by wire cut electrical discharge machining, immersing the iridium crucible into a concentrated sodium hydroxide solution at the temperature of 50-90 ℃, placing the concentrated sodium hydroxide solution into a heatable ultrasonic cleaning machine, carrying out ultrasonic treatment for 10-30 min, then placing the iridium crucible into a vacuum annealing furnace, carrying out heat preservation for 10-30 min at the temperature of 1150-1300 ℃, annealing along with the furnace, then placing the iridium crucible into a magnetic polishing machine for treatment, then placing the iridium crucible into a hydrochloric acid solution with the concentration of 20-38% for heating to boiling, carrying out heat preservation for 10-40 min, cleaning, drying, and then packaging and storing by using a preservative film.
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