CN86108434A - The manufacture method of iridium crucible - Google Patents
The manufacture method of iridium crucible Download PDFInfo
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- CN86108434A CN86108434A CN86108434.9A CN86108434A CN86108434A CN 86108434 A CN86108434 A CN 86108434A CN 86108434 A CN86108434 A CN 86108434A CN 86108434 A CN86108434 A CN 86108434A
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Abstract
The present invention mainly is applicable to the manufacturing field of iridium crucible.The present invention adopts plastic deformation processing method, has solved the defective that temperature field in use is uneven and service life is short low because of iridium crucible density and that the Iridium Crucible wall unevenness is brought.This manufacture method is that argon arc welding and operations such as line cutting, hot spinning and cleaning and polishing are formed by smelting, casting, hot rolling, hot shearing, the bent moulding of hot rolling.Adopting the inventive method can produce diameter is above major diameter, thin-walled iridium crucible of 100mm.
Description
The invention belongs to the manufacture method of iridium material product, be specially adapted to the manufacturing field of iridium crucible.
Because metal iridium has very high intensity and hardness, have again that wearability is good, non-oxidizability is strong, fusing point is high, when high temperature, have characteristics such as antioxygen poisoning and improve the ability of electronics emission.Therefore use vessels crucible when being widely used in the manufacturing crystal growth such as vacuum electronic tube material and costume jewelry and Laser emission material ruby, neodymium-doped yttrium-aluminum garnet.
At present, the method for manufacturing iridium crucible has four kinds.Casting, electrodeposition process, powder compacting method and the plastic working method of forming.Adopt casting method to produce iridium crucible, be with pure iridium powder and metal iridium after the intermediate frequency furnace fusing, directly iridium solution is injected magnesia or graphite mould, cast iridium crucible.Though casting production iridium crucible production technology is simple, and a lot of deficiencies are arranged.Major defect has: the sidewall of crucible thickness ununiformity is even, and wall thickness difference maximum can reach 50%, inner interlayer, loose serious, and the density of crucible has only 18.86g/Cm
3, cause iridium crucible that the seepage phenomenon is often arranged in use, the temperature field inequality is arranged during use, influence the crystal growth quality.Adopt casting can only produce φ 80mm following minor diameter, heavy wall iridium crucible.Adopt the powder compacting method to produce iridium crucible, though manufacture method is simpler, device therefor is very complicated, and the density of iridium crucible is generally 85～90% of solid density behind sintering, also must consider the preparation of raw material simultaneously.Have electrodeposition process can only produce the very thin iridium crucible of minor diameter, wall thickness again, and the density of iridium crucible also is very low, is about about 85% of solid density.But it is very difficult adopting plastic deformation processing method that iridium is processed, because when room temperature, the iridium plate tensile strength of deformation state is 210.9～253.1kgf/mm
2, the iridium plate tensile strength during annealed condition is also up to 112.5～126.5kgf/mm
2The resistance of deformation of iridium also reaches 60kgf/mm when 1200 ℃ of high temperature
2About, plasticity is also very poor.Also have the high-temperature oxydation phenomenon.Therefore, adopt the plastic deformation method to produce the iridium crucible goods.In manufacture method, the process technology difficulty is very big.The manufacture method of relevant iridium crucible goods, also not seeing has any data introduction abroad.
The purpose of this invention is to provide a kind of can the economic density of producing be 22.65g/Cm
3, eliminated interlayer and wall unevenness phenomenon in the goods, the manufacture method of major diameter, thin-walled iridium crucible goods again.
According to above-mentioned requirements, the present invention designs a kind of method of making iridium crucible.This manufacture method is described below: the iridium plate (every heating is once rolling together) that 1200～1500 ℃ on the preparation of raw materials for metallurgy (pure iridium powder, piece or reclaim the iridium piece) → intermediate frequency furnace melting → be cast in the 1600 ℃ of magnesia moulds thick iridium ingot of 20mm → be heated in electric furnace → roll on φ 300mm vacuum rolling mill is set thickness → the roll bent moulding of after-baking → hot shearing → hot rolling → line cutting → argon arc welding → hot spinning → surface clean → polishing.
With regard to the method for above-mentioned manufacturing iridium crucible, every kind of technology and principle are described in detail as follows:
1. the preparation of iridium material: the volatilization of iridium powder and be easy to fusing when reducing melting, should earlier the iridium powder be pressed into needed shape and size specification, the purity of iridium powder is 99.95%, the pressure 2T/mm during moulding
2Adopt when reclaiming the iridium material, should earlier the foreign material that stick on the iridium material be removed totally, with hydrochloric acid the iridium material is handled again.The purity of iridium material is more than 99.9%.
2. the melting of iridium: melting is to carry out in intermediate frequency furnace, and equipment adopts DGF-R-58 type frequency changer, and output frequency is 8600Hz, and peak power output is 50KW.Treating during melting needs insulation 20～30 minutes after the iridium material fusing, rapidly iridium solution is injected the magnesia mould that heats then, treat that the iridium ingot solidifies after, with running water mold and iridium ingot are forced to be cooled to room temperature together.
3. the preparation of magnesia mold: with purity be 99.5% magnesia powder in setting the preparation of granularity ratio, after mixing, mix as binding agent with waterglass again, be placed on ramming process in the punching block.The demoulding behind the low-temperature bake, is put into the Si-Mo rod stove again and slowly is heated to 1600 ℃ after air-dry, and being incubated after 2 hours stove, to be chilled to room temperature standby again.During use the magnesia mold is heated to 1600 ℃, is incubated after 1 hour, just can use by ingot casting.
4. iridium ingot heating: the iridium ingot after the demoulding should be cleared up earlier, check, avoids the iridium ingot surface that pickup is arranged.The iridium ingot is put into the Si-Mo rod stove to be heated to 1200～1500 ℃ of insulations and can to carry out hot rolling after 30 minutes.The iridium ingot has serious oxidative phenomena when rolling temperature is higher than 1500 ℃, can not guarantee the back quality of rolling of goods, the waste that brings the iridium material again.Rolling temperature is lower than 1200 ℃ then can cause rolling difficulty.
5. hot rolling: the density of iridium goods is relevant with deformation extent, and when deformation extent reaches more than 70%, the density of iridium can reach solid density 22.65g/Cm
3, so the employing of the hot rolling technology of this manufacture method is rolling on φ 330mm two-roller reversible formula vacuum rolling mill, mill speed 0.76 meter per second, main motor current is 200KW, every heating is once rolling together, and each reduction ratio is 20～30%, and the total deflection in rolling back should be greater than more than 70%.
6. iridium plate heat treatment: the iridium plate after rolling is put into the Si-Mo rod stove roll post processing, for eliminating because of the rolling unfavorable factors such as some stress that produce.Heat treatment temperature is 1250～1300 ℃, is incubated to carry out shrend after 15～20 minutes.
7. hot shearing: for reducing the hardness and the intensity of iridium plate, the iridium plate can be heated to more than 1000 ℃, cut into the size that requires rapidly after getting material.Shearing is sheared on the QD30-6B multi-purpose punching and shearing machine.
8. the bent moulding of hot rolling: the bent iridium tube of hot rolling is to carry out on the three bending make-up machines of φ 60 * 300mm.In the time of will shearing good iridium plate earlier and be heated to 1000～1100 ℃, take out to send into behind the iridium plate and carry out the hot rolling song on the three bending make-up machines and give moulding, and then be heated to 1000 ℃ to the iridium tube cans of finalizing the design, make interface neat, tight, and the processing that eliminates stress.
9. argon arc welding: welding is to weld on WS-300 type argon arc welding machine; should be during welding earlier to good weld bond and fixing; the iridium bar that scolder adopts the iridium plate to downcut; electric current during welding is 300 amperes; adopt simultaneously and treat that the weld bond temperature reduces to below 100 ℃ after argon shield weldering, the welding, remove protective gas again.Two parallel end faces vertical with the iridium tube are cut into wire cutting machine in iridium tube two ends, add the weldering chassis again, and welding method is identical with preceding paragraph.
10. hot spinning: earlier the iridium crucible goods that weld are enclosed within on the heat resisting steel plug, and with the good workpiece of chuck card, with fuel gas the iridium crucible goods are heated to 800～900 ℃ then, use with the symmetrical two or more spinning wheels of work centre line again and carry out symmetrical hot spinning, every time drafts is 10% of iridium crucible wall thickness and a reinforcement of weld gross thickness.Spinning is smooth smooth up to weld bond, carries out shaping with light reduction at last.The employing hot spinning method carries out the processing to weld bond, can make weld bond become interior tissue identical with iridium crucible and density by former as-cast structure.Make weld bond smooth smooth, for the use of iridium crucible has later on brought convenience.
11. surface clean and polishing: crucible is heated to 1300 ℃, again iridium crucible is put into concentration after the cooling and be 50% hydrochloric acid solution and boil, again with distilled water clean, oven dry.Polishing adopts fabric disc to carry out machine glazed finish.
Adopt method of the present invention, the iridium crucible of manufacturing is compared with the iridium crucible that other method is produced, and has the following advantages:
(1) compare with casting, every iridium crucible can be saved iridium material 30～40%, and annual the need provides 30 above iridium crucibles to domestic, adopts this manufacture method to produce, and can save the about 28kg of iridium material, amounts to surplus the RMB about 1,530,000 yuan.
(2) eliminated the defective such as interlayer, cavity of iridium crucible inside, made crucible density by 18.89g/Cm
3Bring up to solid density 22.65g/Cm
3, the loss that has reduced iridium in use is more than 80%, and improved the surface quality of iridium crucible, prolonged service life of iridium crucible.
(3) reduced the even property of wall unevenness, make wall thickness deviation by ± 25% be reduced to ± 3%, eliminated the inhomogeneities in single crystal growing furnace temperature field when iridium crucible uses, improved the quality of crystalline articles, reduced energy consumption.
(4) compare with other method, adopt this method, can produce density is 22.65g/Cm
3Above major diameter, the thin-walled iridium crucible of φ 100mm.
(5) adopt the comparative result of the iridium crucible performance that manufacture method of the present invention and other method produce to see the following form 1:
The iridium crucible performance of table 1, four kinds of method manufacturings of employing relatively
| Ginseng number formulary method | Density g/cm 3 | Wall thickness deviation | Internal structure | Surface quality | Crucible size | The crucible wall thickness |
| Powder compacting | 19.2 | ±5% | Loose | Generally | Below the φ 120mm | Greater than 3mm |
| Electrodeposition process | 19.2 | ±5% | Loose | Generally | Minor diameter thin wall | Less than 0.5mm |
| Casting | 18.89 | ±25% | Loosening has interlayer | Coarse | Below the φ 80mm | Greater than 3mm |
| The plastic deformation method | 22.65 | ±3% | Fine and close | Well | More than the φ 100mm | 1-3mm |
Embodiment
According to above-mentioned narration to plastic deformation method of the present invention, to the comparison of iridium crucible manufacture method, we have adopted the plastic deformation method to produce φ 100mm, and wall thickness is the iridium crucible of 2.0mm.Specifically production routine is, raw material employing purity is 99.95% iridium powder, and the iridium powder is pressed into pole, and pressure is 2T/mm
2The iridium rod that suppresses is put into the intermediate frequency furnace melting, treat that iridium material fusing back kept 20 minutes, iridium solution is injected 1600 ℃ magnesia mould again, ingot casting is of a size of 20 * 100 * 150mm, after the iridium ingot solidified, water forced to be cooled to room temperature together with mold and iridium ingot.Wash impurity, cleaning, drying again off with the hydrochloric acid heating of 50% concentration again after taking out the iridium ingot.The iridium ingot is put into stove be heated to 1300 ℃ of insulations after 30 minutes, carry out hot rolling on φ 330mm two roller vacuum rolling mills, reduction per pass is 20%, whenever rolls one heating once, and to be rolled to thickness be the thick iridium plate of 2mm to the iridium ingot the most at last.The iridium plate is heat-treated, temperature is 1250 ℃ of insulation shrends after 15 minutes again.Send into the QD30-6B multi-purpose punching and shearing machine after again the iridium plate being heated to 1000 ℃ and cut edge forming.Put into φ 60 * 300mm three bending make-up machines after the iridium plate that cuts is heated to 1100 ℃ and give moulding and curl, again the iridium tube is melted down and be heated to 1000 ℃ and eliminate stress, and divide five roads to finalize the design to curl and make the interface alignment.The iridium tube that interface is alignd is fixed on the WS-300 type argon arc welding machine and welds at last, adopts argon shield during welding, welds the back and carry out two ends processing on wire cutting machine, adds the weldering chassis after the processing again, and welding method is identical with preceding paragraph.The iridium crucible that welds is enclosed within on the heat resisting steel plug and with chuck card jail again, carries out hot spinning after with the method for coal gas heating iridium crucible being heated to 850 ℃, spinning is smooth for suitable to the iridium crucible weld bond.Iridium crucible behind the spinning is heated to 1300 ℃ again and puts into 50% hydrochloric acid solution after cooling and boil, and pulls out after acid is boiled again and cleans, dries.Carry out machine glazed finish with fabric disc again.
Claims (5)
1, a kind of manufacture method of iridium crucible wherein includes melting, casting, hot shearing and surface clean and polishing process, it is characterized in that processing by heating rolling, welding and hot spinning the manufacture method of the iridium crucible of being produced.
According to the described method of claim 1, it is characterized in that 2, the hot rolling heating-up temperature is 1200～1500 ℃.
3,, it is characterized in that every rolling heating together once, but the total deformation of hot rolling system is greater than 70% according to the described method of claim 1.
4, according to the described method of claim 1, the heating-up temperature that it is characterized in that hot spinning is 800 ℃-900 ℃.
5,, it is characterized in that every time drafts of hot spinning is 10% of crucible wall thickness and a reinforcement of weld sum according to claim 1,4 described methods.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86108434.9A CN1003733B (en) | 1986-12-20 | 1986-12-20 | Method for making iridium crucible |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86108434.9A CN1003733B (en) | 1986-12-20 | 1986-12-20 | Method for making iridium crucible |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86108434A true CN86108434A (en) | 1988-08-10 |
| CN1003733B CN1003733B (en) | 1989-03-29 |
Family
ID=4803922
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN86108434.9A Expired CN1003733B (en) | 1986-12-20 | 1986-12-20 | Method for making iridium crucible |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1003733B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102989856A (en) * | 2012-12-03 | 2013-03-27 | 西安西工大超晶科技发展有限责任公司 | Method for molding large variable-wall-thickness pure molybdenum crucible |
| CN104668909A (en) * | 2015-02-05 | 2015-06-03 | 北京华夏富润工贸有限公司 | High-precision weldless iridium crucible and manufacturing method of iridium products |
| CN106270462A (en) * | 2016-08-01 | 2017-01-04 | 陕西三毅有岩材料科技有限公司 | A kind of preparation method casting iridium crucible |
| CN108421824A (en) * | 2018-03-12 | 2018-08-21 | 陕西三毅有岩材料科技有限公司 | Iridium plate and its processing method, iridium crucible |
| CN108580549A (en) * | 2018-03-14 | 2018-09-28 | 陕西三毅有岩材料科技有限公司 | A kind of crucible of iridium plate and its processing method and preparation |
| CN111085827A (en) * | 2019-12-26 | 2020-05-01 | 无锡英特派金属制品有限公司 | Method for manufacturing large-size high-density bright iridium crucible |
| CN114029709A (en) * | 2021-12-03 | 2022-02-11 | 中国工程物理研究院核物理与化学研究所 | Forming method of iridium alloy sealing cladding |
-
1986
- 1986-12-20 CN CN86108434.9A patent/CN1003733B/en not_active Expired
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102989856A (en) * | 2012-12-03 | 2013-03-27 | 西安西工大超晶科技发展有限责任公司 | Method for molding large variable-wall-thickness pure molybdenum crucible |
| CN102989856B (en) * | 2012-12-03 | 2014-12-10 | 西安超晶新能源材料有限公司 | Method for molding large variable-wall-thickness pure molybdenum crucible |
| CN104668909A (en) * | 2015-02-05 | 2015-06-03 | 北京华夏富润工贸有限公司 | High-precision weldless iridium crucible and manufacturing method of iridium products |
| CN104668909B (en) * | 2015-02-05 | 2017-02-22 | 北京华夏富润工贸有限公司 | Manufacturing method of high-precision weldless iridium crucible |
| CN106270462A (en) * | 2016-08-01 | 2017-01-04 | 陕西三毅有岩材料科技有限公司 | A kind of preparation method casting iridium crucible |
| CN108421824A (en) * | 2018-03-12 | 2018-08-21 | 陕西三毅有岩材料科技有限公司 | Iridium plate and its processing method, iridium crucible |
| CN108580549A (en) * | 2018-03-14 | 2018-09-28 | 陕西三毅有岩材料科技有限公司 | A kind of crucible of iridium plate and its processing method and preparation |
| CN111085827A (en) * | 2019-12-26 | 2020-05-01 | 无锡英特派金属制品有限公司 | Method for manufacturing large-size high-density bright iridium crucible |
| CN114029709A (en) * | 2021-12-03 | 2022-02-11 | 中国工程物理研究院核物理与化学研究所 | Forming method of iridium alloy sealing cladding |
| CN114029709B (en) * | 2021-12-03 | 2023-02-03 | 中国工程物理研究院核物理与化学研究所 | Forming method of iridium alloy sealing cladding |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1003733B (en) | 1989-03-29 |
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