CN102786313B - Dry-type preparation method of self-sintering magnesium oxide crucible of vacuum induction furnace - Google Patents
Dry-type preparation method of self-sintering magnesium oxide crucible of vacuum induction furnace Download PDFInfo
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- CN102786313B CN102786313B CN201210300851.9A CN201210300851A CN102786313B CN 102786313 B CN102786313 B CN 102786313B CN 201210300851 A CN201210300851 A CN 201210300851A CN 102786313 B CN102786313 B CN 102786313B
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Abstract
The invention discloses a dry-type preparation method of self-sintering magnesium oxide crucible of a vacuum induction furnace. The dry-type preparation method orderly comprises the following steps of: paving a backing material inside a copper round induction tube bundle of the induction furnace; adding a crucible furnace construction material into the copper round induction tube bundle; constructing and tamping to form a furnace bottom; putting a graphite tire core into the copper round induction tube bundle, and keeping the axes of the graphite tire core and the copper round induction tube bundle overlapped; adding the furnace construction material into a gap in the periphery of the graphite tire core, gradually constructing and tamping to form a furnace body, adding a furnace opening material when the height of the furnace body is constructed and tamped to 1-2 rows from an upper opening of the copper round induction tube bundle, constructing and tamping the material to form a furnace opening; and supplying electricity to the copper round induction tube bundle to be baked, closing a vacuum room of the induction furnace, vacuumizing and charging argon to seal, sintering for 1-2 hours, adding a steel material for toughening the furnace, and washing the furnace. The magnesium oxide crucible prepared by the method is short in preparation process period, high in energy consumption and long in furnace life.
Description
Technical field
The invention belongs to crucible preparation method technical field, specifically refer to the dry type making method of a kind of vacuum induction furnace from the magnesia crucible of sintering oxidation.
Background technology
Tradition prepares multiplex wet method from the magnesia crucible of sintering oxidation, as the Chinese invention patent that application number is 200910064477.5, discloses a kind of making method of aluminium titanate crucible product, and described making method is: the mass percent by following raw material is prepared burden: Al
2o
350 ~ 57%, TiO
237 ~ 44%, additive (MgO, BaO, Y
2o
3, La
2o
3) 6 ~ 8%; The additional wedding agent aqueous solution (acrylamide, double focusing acrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine and water) 18 ~ 23% again after batching is mixed is made slurry in ball mill or stirrer; Slurry is injected in the goods mould, after solidifying, base substrate is taken out from mould; Base substrate is packed in the baking oven that temperature is 80 ~ 100 ℃, be incubated 30 ~ 40h and dry; To dry base substrate and pack in the high temperature kiln that temperature is 1550 ~ 1630 ℃, and be incubated 4 ~ 10h and carry out sintering.But, because its additive is the aqueous solution, spice difficulty labour intensity is large, and is difficult for mixing thoroughly; Health after corresponding shaping, baking, even prepurging complex process of sintering, time is long, energy consumption is large, efficiency is low, steam in crucible is difficult to timely discharge, sometimes smelts in the above vacuum chamber of 6 stove vacuum tightness also more than 10Pa, makes furnace life front 6 ~ 10 stoves can't smelt Clean Steel, the organization of production difficulty, the useless rate of refining is high; Discharge a large amount of steam while especially playing after the type of building up baking, prepurging, can't carry out in vacuum chamber, magnesium oxide inevitable with atmosphere in carbon dioxide reaction affect crucible life.
Summary of the invention
Purpose of the present invention is exactly that the dry type making method of a kind of vacuum induction furnace from the magnesia crucible of sintering oxidation will be provided, and the magnesia crucible preparation technology cycle that the method is made is short, energy consumption is high, furnace life is long.
For achieving the above object, vacuum induction furnace of the present invention, from the dry type making method of the magnesia crucible of sintering oxidation, comprises the following steps successively:
1) lay one deck priming material in the induction copper coin pipe of induction furnace is arranged after, in induction copper coin pipe row, add the crucible furnace building material, beat and build compacting formation furnace bottom;
2) put into graphite tire core in induction copper coin pipe row, and keep graphite tire core and the axis coinciding of responding to copper coin pipe row;
3) gap to graphite tire core periphery adds the brickwork material, successively beats and builds compacting, forms body of heater;
4) the body of heater height is beaten and is built while to induction copper coin pipe, arranging 1 ~ 2 row suitable for reading, adds the fire door material, beats and builds compacting, forms fire door;
5) give induction copper coin pipe dispatch electricity, with 50 ~ 250 ℃ of baking 1 ~ 2h, then with 250 ~ 1650 ℃ of baking 6 ~ 8h;
6) the induction furnace vacuum chamber that closes, first be evacuated to 50 ~ 80Pa, then argon filling carries out the argon envelope, with 1600 ~ 1750 ℃ of sintering 1 ~ 2h;
7) add the prepurging of steel material steel to complete;
Wherein, in described crucible furnace building material, the weight percent content of each component is: the electrically molten magnesia sand of 0mm<granularity≤5mm accounts for 60 ~ 90%, the electrically molten magnesia sand of 5mm<granularity≤8mm accounts for 5 ~ 35%, the calcium oxide of 0mm<granularity≤1mm accounts for 1 ~ 3%, the lapis amiridis of 0mm<granularity≤1mm accounts for 0.1 ~ 0.5%, the boric acid powder of 0mm<granularity≤1mm accounts for 1 ~ 3%;
The paste-like material that adds the industrial spirit modulation of purity more than 99% to form after the boric acid powder that described fire door material is by weight percentage is 2 ~ 5% by 95 ~ 98% magnesium oxide sand and weight ratio mixes, described magnesium oxide sand and boric acid powder all meet 0<granularity≤1mm.
Preferably, in described step 1), priming material is woven asbesto or glasscloth.
Further, beating brickwork base thickness degree described step 2) is 5 ~ 50mm.
Again further, while toasting in described step 5), Open Side Down on induction copper coin pipe row top tilts 30 ~ 60 °, that moisture that fire door is discharged directly drips and is easy to discharge like this, if the moisture that fire door is discharged during vertical crucible heating can be difficult to discharge along the dirty body of heater absorbed be dried again of body of heater.
Vacuum induction furnace of the present invention is as follows from the principle of operation of each step of dry type making method of the magnesia crucible of sintering oxidation:
Making method of the present invention adopts electrically molten magnesia sand to make major ingredient, adopts boric acid powder and calcium oxide, lapis amiridis as main caking agent, plays the effect of caking agent and reinforcer at low thermophase boric acid, at hot stage MgO+CaO+Al
2o
3chemical reaction occurs, CaO+Al
2o
3play the effect of caking agent, thereby guaranteed the intensity of crucible.The moisture that 250 ℃ of boric acid powders resolve into anhydride and boric acid decomposes seldom, is played the alcohol of brickwork mouth use and is very easily discharged, thereby make the oven drying time greatly shorten, and the crucible preparation technology cycle also just significantly reduces, energy consumption also significantly reduces.Traditional manufacturing technique is all to open wide in atmosphere to be toasted sintering, the time that a large amount of steam is discharged is long, can damage vacuum pump in vacuum chamber, and manufacture craft of the present invention adopts omnidistance waterless operation, batching and to beat the process of building anhydrous, dry baking of short period of time steam is discharged very soon like this, makes on technique and can make fast crucible argon envelope in vacuum chamber carry out high bake and sintering, CO in atmosphere while having avoided high temperature
2react with MgO on sidewall of crucible, thereby guaranteed the quality of sidewall of crucible, improved crucible life.Simultaneously, due to dry type, anhydrous preparation technology makes steam few, and in vacuum chamber, vacuum tightness can improve fast, and significantly shift to an earlier date the opportunity of smelting ultra-clean steel, and the scrap rate of smelting ultra-clean steel reduces.In vacuum chamber, under argon envelope state, carry out, the interior vacuum tightness of front 2 stove vacuum chambers of furnace life can reach below 1Pa, and the 3rd stove can start to smelt ultra-clean steel.Thereby, the advantages such as preparation method of the present invention has that crucible life is long, with low cost, work simplification, organization of production are simple, high-efficient energy-saving environment friendly, be suitable for laboratory or pilot plant and buy the large-scale crucible that prefabricated crucible is difficult for keeping and integrated mill and be difficult for buying the occasions such as the prefabricated crucible of transportation.
Embodiment
Below in conjunction with specific embodiment, to vacuum induction furnace of the present invention, the dry type making method from the magnesia crucible of sintering oxidation is described in further detail.
Embodiment 1
1) lay one deck woven asbesto in the induction copper coin pipe of induction furnace is arranged after, in induction copper coin pipe row, add the crucible furnace building material, beat and build compacting formation furnace bottom, furnace bottom thickness is 15mm;
2) put into graphite tire core in induction copper coin pipe row, and keep graphite tire core and induction copper coin pipe to arrange both axis coincidings;
3) gap to graphite tire core periphery adds the brickwork material, successively beats and builds compacting, forms body of heater;
4) the body of heater height is beaten and is built while to induction copper coin pipe, arranging 1 row suitable for reading, adds the fire door material, beats and builds compacting, forms fire door;
5) give induction copper coin pipe dispatch electricity, with 50 ~ 250 ℃ of baking 2h, fire door alcohol and steam that may be remaining are volatilized fully, then with 250 ~ 1650 ℃ of baking 8h, during baking, Open Side Down on induction copper coin pipe row top tilts 35 °;
6) the induction furnace vacuum chamber that closes, first be evacuated to 50 ~ 80Pa, then applying argon gas carries out the argon envelope, with 1750 ℃ of sintering 2h;
7) take out the crucible of sintering, add the prepurging of steel material steel to complete;
Wherein, in described crucible furnace building material, the weight percent content of each component is: the electrically molten magnesia sand of 0mm<granularity≤5mm accounts for 60%, the electrically molten magnesia sand of 5mm<granularity≤8mm accounts for 35%, the calcium oxide of 0mm<granularity≤1mm accounts for 2.5%, the lapis amiridis of 0mm<granularity≤1mm accounts for 0.5%, the boric acid powder of 0mm<granularity≤1mm accounts for 2%;
The paste-like material that adds the industrial spirit modulation of purity more than 99% to form after the boric acid powder that the magnesium oxide sand that described fire door material is is 95% by weight ratio and weight ratio are 5% mixes, described magnesium oxide sand and boric acid powder all meet 0<granularity≤1mm.
Effect: in preparation process, furnace drying time amounts to 12 hours, and (and use before the present invention, adopting the average furnace drying time 24 hours that traditional wet method makes) shortens 50%; The interior vacuum tightness of front 2 stove vacuum chambers of furnace life can reach 0.9Pa, and the 3rd stove can start to smelt ultra-clean steel, and (and average the 10th stove of crucible that adopts traditional wet method to make just can be smelted ultra-clean steel reluctantly) shifts to an earlier date 70% opportunity; Crucible life 80 stoves, (common crucible mean lifetime 50 stoves) extend 60%.
Embodiment 2
1) lay layer of glass cloth in the induction copper coin pipe of induction furnace is arranged after, in induction copper coin pipe row, add the crucible furnace building material, beat and build compacting formation furnace bottom, furnace bottom thickness is 50mm;
2) put into graphite tire core in induction copper coin pipe row, and keep graphite tire core and induction copper coin pipe to arrange both axis coincidings;
3) gap to graphite tire core periphery adds the brickwork material, successively beats and builds compacting, forms body of heater;
4) the body of heater height is beaten and is built while to induction copper coin pipe, arranging 2 row suitable for reading, adds the fire door material, beats and builds compacting, forms fire door;
5) give induction copper coin pipe dispatch electricity, with 50 ~ 250 ℃ of baking 1.5h, fire door alcohol and steam that may be remaining are volatilized fully, then with 250 ~ 1650 ℃ of baking 8h, during baking, Open Side Down on induction copper coin pipe row top tilts 45 °;
6) the induction furnace vacuum chamber that closes, first be evacuated to 50 ~ 80Pa, then argon filling carries out the argon envelope, with 1600 ℃ of sintering 1.5h;
7) take out the crucible of sintering, add the prepurging of steel material steel to complete;
Wherein, in described crucible furnace building material, the weight percent content of each component is: the electrically molten magnesia sand of 0mm<granularity≤5mm accounts for 90%, the electrically molten magnesia sand of 5mm<granularity≤8mm accounts for 5%, the calcium oxide of 0mm<granularity≤1mm accounts for 2%, the lapis amiridis of 0mm<granularity≤1mm accounts for 0.5%, the boric acid powder of 0mm<granularity≤1mm accounts for 2.5%;
The paste-like material that adds the industrial spirit modulation of purity more than 99% to form after the boric acid powder that the magnesium oxide sand that described fire door material is is 98% by weight ratio and weight ratio are 2% mixes, this magnesium oxide sand and boric acid powder all meet 0<granularity≤1mm.
Effect: in preparation process, furnace drying time amounts to 11 hours, shortens 54%; The interior vacuum tightness of front 2 stove vacuum chambers of furnace life can reach 0.8Pa, and the 3rd stove can start to smelt ultra-clean steel, and shift to an earlier date 60% opportunity; Crucible life 82 stoves, extend 64%.
Embodiment 3
1) lay one deck woven asbesto in the induction copper coin pipe of induction furnace is arranged after, in induction copper coin pipe row, add the crucible furnace building material, beat and build compacting formation furnace bottom, furnace bottom thickness is 30mm;
2) put into graphite tire core in induction copper coin pipe row, and keep graphite tire core and induction copper coin pipe to arrange both axis coincidings;
3) gap to graphite tire core periphery adds the brickwork material, successively beats and builds compacting, forms body of heater;
4) the body of heater height is beaten and is built while to induction copper coin pipe, arranging 2 row suitable for reading, adds the fire door material, beats and builds compacting, forms bright and clean fire door;
5) give induction copper coin pipe dispatch electricity, with 50 ~ 250 ℃ of baking 2h, fire door alcohol and steam that may be remaining are volatilized fully, then with 250 ~ 1650 ℃ of baking 8h, during baking, Open Side Down on induction copper coin pipe row top tilts 50 °;
6) the induction furnace vacuum chamber that closes, first be evacuated to 67Pa, then applying argon gas carries out the argon envelope, with 1700 ℃ of sintering 2h;
7) take out the crucible of sintering, add the prepurging of steel material steel to complete;
Wherein, in described crucible furnace building material, the weight percent content of each component is: the electrically molten magnesia sand of 0mm<granularity≤5mm accounts for 85%, the electrically molten magnesia sand of 5mm<granularity≤8mm accounts for 10%, the calcium oxide of 0mm<granularity≤1mm accounts for 2.5%, the lapis amiridis of 0mm<granularity≤1mm accounts for 0.5%, the boric acid powder of 0mm<granularity≤1mm accounts for 2%;
The paste-like material that adds the industrial spirit modulation of purity more than 99% to form after the boric acid powder that the magnesium oxide sand that described fire door material is is 98% by weight ratio and weight ratio are 2% mixes, this magnesium oxide sand and boric acid powder all meet 0<granularity≤1mm.
Effect: furnace drying time amounts to 12 hours, shortens 50%; The interior vacuum tightness of front 2 stove vacuum chambers of furnace life can reach 0.9Pa, and the 3rd stove can start to smelt ultra-clean steel, and shift to an earlier date 70% opportunity; Crucible life 78 stoves, extend 56%.
Embodiment 4
1) lay one deck woven asbesto in the induction copper coin pipe of induction furnace is arranged after, in induction copper coin pipe row, add the crucible furnace building material, beat and build compacting formation furnace bottom, furnace bottom thickness is 25mm;
2) put into graphite tire core in induction copper coin pipe row, and keep graphite tire core and induction copper coin pipe to arrange both axis coincidings;
3) gap to graphite tire core periphery adds the brickwork material, successively beats and builds compacting, forms body of heater;
4) the body of heater height is beaten and is built while to induction copper coin pipe, arranging 1 row suitable for reading, adds the fire door material, beats and builds compacting, forms bright and clean fire door;
5) give induction copper coin pipe dispatch electricity, with 50 ~ 250 ℃ of baking 1.5h, fire door alcohol and steam that may be remaining are volatilized fully, then with 250 ~ 1650 ℃ of baking 7.5h, during baking, Open Side Down on induction copper coin pipe row top tilts 60 °;
6) the induction furnace vacuum chamber that closes, first be evacuated to 67Pa, then argon filling carries out the argon envelope, with 1750 ℃ of sintering 2h;
7) take out the crucible of sintering, add the prepurging of steel material steel to complete;
Wherein, in described crucible furnace building material, the weight percent content of each component is: the electrically molten magnesia sand of 0mm<granularity≤5mm accounts for 88%, the electrically molten magnesia sand of 5mm<granularity≤8mm accounts for 8%, the calcium oxide of 0mm<granularity≤1mm accounts for 1.5%, the lapis amiridis of 0mm<granularity≤1mm accounts for 0.5%, the boric acid powder of 0mm<granularity≤1mm accounts for 2%;
The paste-like material that adds the industrial spirit modulation of purity more than 99% to form after the boric acid powder that the magnesium oxide sand that described fire door material is is 98.5% by weight ratio and weight ratio are 1.5% mixes, this magnesium oxide sand and boric acid powder all meet 0<granularity≤1mm.
Effect: furnace drying time amounts to 11 hours, shortens 54%; The interior vacuum tightness of front 2 stove vacuum chambers of furnace life can reach 0.8Pa, and the 3rd stove can start to smelt ultra-clean steel, and shift to an earlier date 60% opportunity; Crucible life 82 stoves, extend 64%.
Embodiment 5
1) lay one deck woven asbesto in the induction copper coin pipe of induction furnace is arranged after, in induction copper coin pipe row, add the crucible furnace building material, beat and build compacting formation furnace bottom, furnace bottom thickness is 40mm;
2) put into graphite tire core in induction copper coin pipe row, and keep graphite tire core and induction copper coin pipe to arrange both axis coincidings;
3) gap to graphite tire core periphery adds the brickwork material, successively beats and builds compacting, forms body of heater;
4) the body of heater height is beaten and is built while to induction copper coin pipe, arranging 1 row suitable for reading, adds the fire door material, beats and builds compacting, forms bright and clean fire door;
5) give induction copper coin pipe dispatch electricity, with 50 ~ 250 ℃ of baking 2h, fire door alcohol and steam that may be remaining are volatilized fully, then with 250 ~ 1650 ℃ of baking 7h, during baking, Open Side Down on induction copper coin pipe row top tilts 40 °;
6) the induction furnace vacuum chamber that closes, first be evacuated to 67Pa, then argon filling carries out the argon envelope, with 1750 ℃ of sintering 1.5h;
7) take out the crucible of sintering, add the prepurging of steel material steel to complete;
Wherein, in described crucible furnace building material each component by weight percent content, be: the electrically molten magnesia sand of 0mm<granularity≤5mm accounts for 87%, the electrically molten magnesia sand of 5mm<granularity≤8mm accounts for 10%, the calcium oxide of 0mm<granularity≤1mm accounts for 1.5%, the lapis amiridis of 0mm<granularity≤1mm accounts for 0.5%, the boric acid powder of 0mm<granularity≤1mm accounts for 1%;
The paste-like material that adds the industrial spirit modulation of purity more than 99% to form after the boric acid powder that the magnesium oxide sand that described fire door material is is 97% by weight ratio and weight ratio are 3% mixes, this magnesium oxide sand and boric acid powder all meet 0<granularity≤1mm.
Effect: furnace drying time amounts to 10.5 hours, shortens 56%; The interior vacuum tightness of front 2 stove vacuum chambers of furnace life can reach 0.75Pa, and the 3rd stove can start to smelt ultra-clean steel, and shift to an earlier date 60% opportunity; Crucible life 79 stoves, extend 58%.
Claims (3)
1. a vacuum induction furnace is from the dry type making method of the magnesia crucible of sintering oxidation, and it is characterized in that: it comprises the following steps successively:
1) lay one deck priming material in the induction copper coin pipe of induction furnace is arranged after, in induction copper coin pipe row, add the crucible furnace building material, beat and build compacting formation furnace bottom;
2) put into graphite tire core in induction copper coin pipe row, and keep graphite tire core and the axis coinciding of responding to copper coin pipe row;
3) gap to graphite tire core periphery adds the brickwork material, successively beats and builds compacting, forms body of heater;
4) the body of heater height is beaten and is built while to induction copper coin pipe, arranging 1 ~ 2 row suitable for reading, adds the fire door material, beats and builds compacting, forms fire door;
5) give induction copper coin pipe dispatch electricity, with 50 ~ 250 ℃ of baking 1 ~ 2h, then with 250 ~ 1650 ℃ of baking 6 ~ 8h, during baking, Open Side Down on induction copper coin pipe row top tilts 30 ~ 60 °;
6) the induction furnace vacuum chamber that closes, first be evacuated to 50 ~ 80Pa, then applying argon gas carries out the argon envelope, with 1600 ~ 1750 ℃ of sintering 1 ~ 2h;
7) add the prepurging of steel material steel to complete;
Wherein, in described crucible furnace building material, the weight percent content of each component is: the electrically molten magnesia sand of 0mm<granularity≤5mm accounts for 60 ~ 90%, the electrically molten magnesia sand of 5mm<granularity≤8mm accounts for 5 ~ 35%, the calcium oxide of 0mm<granularity≤1mm accounts for 1 ~ 3%, the lapis amiridis of 0mm<granularity≤1mm accounts for 0.1 ~ 0.5%, the boric acid powder of 0mm<granularity≤1mm accounts for 1 ~ 3%;
Described fire door material is the paste-like material that adds the industrial spirit modulation of purity more than 99% to form after the boric acid powder by 95 ~ 98% magnesium oxide sand and 2 ~ 5% mixes by weight percentage, and described magnesium oxide sand and boric acid powder all meet 0<granularity≤1mm.
2. vacuum induction furnace, from the dry type making method of the magnesia crucible of sintering oxidation, is characterized in that according to claim 1: in described step 1), priming material is woven asbesto or glasscloth.
3. the dry type making method from the magnesia crucible of sintering oxidation according to the described vacuum induction furnace of claim 1 or 2, it is characterized in that: in described step 1), beating brickwork base thickness degree is 5 ~ 50mm.
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CN103121852B (en) * | 2012-12-12 | 2014-07-16 | 上海电气钠硫储能技术有限公司 | Magnesia crucible for synthesizing sodium-sulfur cell solid electrolyte and preparation method of magnesia crucible |
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CN111023806A (en) * | 2019-11-25 | 2020-04-17 | 包头钢铁(集团)有限责任公司 | Preparation method of crucible for 25kg vacuum induction furnace |
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CN112321282B (en) * | 2020-11-05 | 2022-04-12 | 山东瑞泰新材料科技有限公司 | High-strength magnesium oxide crucible and preparation method thereof |
CN114410994B (en) * | 2021-12-30 | 2023-07-25 | 北京科技大学 | Based on CaO-MgO-Al 2 O 3 Method for smelting nickel-base superalloy by refractory material |
CN115231916B (en) * | 2022-07-13 | 2023-08-15 | 西安西工大思强科技股份有限公司 | Magnesia-alumina spinel forming crucible and manufacturing method thereof |
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CN101644534B (en) * | 2008-08-08 | 2011-06-22 | 中国科学院金属研究所 | Method for preparing large-capacity calcareous crucible for vacuum induction furnace |
CN101525243A (en) * | 2009-03-26 | 2009-09-09 | 洛阳北苑特种陶瓷有限公司 | Manufacture method for aluminium titanate crucible product |
CN101666580B (en) * | 2009-09-24 | 2012-07-18 | 山西太钢不锈钢股份有限公司 | Manufacturing method of crucible for vacuum induction melting |
CN102192649B (en) * | 2010-10-15 | 2015-08-19 | 株洲中航动力精密铸造有限公司 | A kind of crucible basket for vacuum melting furnace and preparation method thereof |
CN102261841B (en) * | 2011-08-11 | 2013-02-13 | 南通汉瑞实业有限公司 | Crucible cover, manufacturing method thereof and crucible furnace provided with crucible cover |
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