CN102786313A - 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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- CN102786313A CN102786313A CN2012103008519A CN201210300851A CN102786313A CN 102786313 A CN102786313 A CN 102786313A CN 2012103008519 A CN2012103008519 A CN 2012103008519A CN 201210300851 A CN201210300851 A CN 201210300851A CN 102786313 A CN102786313 A CN 102786313A
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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 be meant the dry type making method of a kind of vacuum induction furnace from the magnesia crucible of sintering oxidation.
Background technology
Tradition is from the magnesia crucible of the sintering oxidation preparation wet methods of using more, is 200910064477.5 Chinese invention patent like application number, discloses a kind of making method of aluminium titanate crucible product, and said 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%; Batch mixes is added the wedding agent aqueous solution (acrylic amide, double focusing acrylic amide, ammonium persulphate, Tetramethyl Ethylene Diamine and water) 18 ~ 23% after evenly again, in ball mill or stirrer, process slurry; Slurry is injected in the goods mould, after waiting to solidify base substrate is taken out from mould; With the base substrate temperature of packing into is in 80 ~ 100 ℃ the baking oven, insulation 30 ~ 40h oven dry; To dry the base substrate temperature of packing into is in 1550 ~ 1630 ℃ the high temperature kiln, and insulation 4 ~ 10h carries out sintering.But because its additive is the aqueous solution, spice difficulty labour intensity is big, and is difficult for mixing thoroughly; Health after the corresponding shaping, baking, sintering even prepurging complex process, the time is long, and energy consumption is big; Efficient is low; Steam in the crucible is difficult to timely discharge, smelts in the above Vakuumkammer of 6 stoves vacuum tightness sometimes also more than 10Pa, makes furnace life preceding 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 when especially playing behind the type of building up baking, prepurging, can't in Vakuumkammer, carry out, Natural manganese dioxide inevitable with atmosphere in carbon dioxide reaction influence crucible life.
Summary of the invention
The object of the 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 this method is made is short, energy consumption is high, furnace life is long.
For realizing above-mentioned purpose, vacuum induction furnace of the present invention may further comprise the steps from the dry type making method of the magnesia crucible of sintering oxidation successively:
1) in the induction copper coin pipe row of induction furnace, behind laying one deck priming material, in induction copper coin pipe row, adds the crucible furnace building material, beat and build compacting formation furnace bottom;
2) in induction copper coin pipe row, put into graphite tire core, and keep graphite tire core and the axis coinciding of responding to copper coin pipe row;
3) add the brickwork material to the gap of graphite tire core periphery, successively beat and build compacting, form body of heater;
4) the body of heater height is beaten and is built when induction copper coin pipe is arranged 1 ~ 2 row suitable for reading, adds the fire door material, beats and builds compacting, the formation fire door;
5) give induction copper coin pipe dispatch electricity, with 50 ~ 250 ℃ of baking 1 ~ 2h, again with 250 ~ 1650 ℃ of baking 6 ~ 8h;
6) the induction furnace Vakuumkammer that closes is evacuated to 50 ~ 80Pa earlier, and argon filling carries out the argon envelope again, with 1600 ~ 1750 ℃ of sintering 1 ~ 2h;
7) adding the prepurging of steel material steel can accomplish;
Wherein, the weight percent content of each component is in the said crucible furnace building material: 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 quicklime 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%;
Said fire door material is to be that 2 ~ 5% boric acid powder mixes the back and adds the paste-like material that the industrial spirit modulation of purity 99% or more forms, all satisfied 0＜granularity of said magnesium oxide sand and boric acid powder≤1mm by 95 ~ 98% magnesium oxide sand and weight ratio by weight percentage.
Preferably, priming material is woven asbesto or glasscloth in the said step 1).
Further, beating brickwork base thickness degree said step 2) is 5 ~ 50mm.
Again further; When toasting in the said step 5); Open Side Down on induction copper coin pipe row top tilts 30 ~ 60 °; Be 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 the heating of vertical crucible can be difficult to discharge along the dirty body of heater absorbed that is dried again of body of heater.
Vacuum induction furnace of the present invention is following 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 quicklime, lapis amiridis as main caking agent, plays the effect of caking agent and reinforcer hanging down thermophase boric acid, at hot stage MgO+CaO+Al
2O
3Chemical reaction takes place, CaO+Al
2O
3Play the effect of caking agent, thereby guaranteed the intensity of crucible.The moisture that 250 ℃ of boric acid powders promptly resolve into anhydride and boric acid decomposes is seldom played the alcohol of brickwork mouth usefulness and is very easily discharged, thereby make the oven drying time shorten greatly, and the crucible preparation technology cycle also just significantly reduces, energy consumption also significantly reduces.Traditional manufacturing technique all is to open wide in the atmosphere to toast sintering; The time that a large amount of steam are discharged is long, in Vakuumkammer, can damage vacuum pump, 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 that crucible argon in Vakuumkammer is sealed on the technology carries out high bake and sintering, CO in the atmosphere when having avoided high temperature
2With MgO reaction on the sidewall of crucible, thereby guarantee the quality of sidewall of crucible, improved crucible life.Simultaneously, because the anhydrous preparation technology of dry type makes steam few, vacuum tightness can improve fast in the Vakuumkammer, 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 Vakuumkammer, carry out under the argon envelope state, the interior vacuum tightness of preceding 2 stove Vakuumkammers of furnace life can reach below the 1Pa, and the 3rd stove can begin to smelt ultra-clean steel.Thereby; 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 are 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 occasions such as the prefabricated crucible of transportation.
Embodiment
Below in conjunction with specific embodiment vacuum induction furnace of the present invention is done further explain from the dry type making method of the magnesia crucible of sintering oxidation.
Embodiment 1
1) in the induction copper coin pipe row of induction furnace, behind laying one deck woven asbesto, 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) in induction copper coin pipe row, put into graphite tire core, and keep graphite tire core and both axis coincidings of induction copper coin pipe row;
3) add the brickwork material to the gap of graphite tire core periphery, successively beat and build compacting, form body of heater;
4) the body of heater height is beaten and is built when induction copper coin pipe is arranged 1 row suitable for reading, adds the fire door material, beats and builds compacting, the formation fire door;
5) give induction copper coin pipe dispatch electricity, make fire door alcohol and possibly volatilize fully by remaining steam with 50 ~ 250 ℃ of baking 2h, again with 250 ~ 1650 ℃ of baking 8h, Open Side Down on induction copper coin pipe row top during baking tilts 35 °;
6) the induction furnace Vakuumkammer that closes is evacuated to 50 ~ 80Pa earlier, and applying argon gas carries out the argon envelope again, with 1750 ℃ of sintering 2h;
7) take out the agglomerating crucible, adding the prepurging of steel material steel can accomplish;
Wherein, the weight percent content of each component is in the said crucible furnace building material: 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 quicklime 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%;
Said fire door material is to be that 95% magnesium oxide sand and weight ratio are that 5% boric acid powder mixes the back and adds the paste-like material that the industrial spirit modulation of purity 99% or more forms, all satisfied 0＜granularity of said magnesium oxide sand and boric acid powder≤1mm by weight ratio.
Effect: in the preparation process, furnace drying time amounts to 12 hours, and (adopting the average furnace drying time 24 hours that traditional wet makes before the present invention and use) shortens 50%; The interior vacuum tightness of preceding 2 stove Vakuumkammers of furnace life can reach 0.9Pa, and the 3rd stove can begin to smelt ultra-clean steel, and (and average the 10th stove of crucible that adopts traditional wet 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) prolong 60%.
Embodiment 2
1) in the induction copper coin pipe row of induction furnace, behind the laying layer of glass cloth, 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) in induction copper coin pipe row, put into graphite tire core, and keep graphite tire core and both axis coincidings of induction copper coin pipe row;
3) add the brickwork material to the gap of graphite tire core periphery, successively beat and build compacting, form body of heater;
4) the body of heater height is beaten and is built when induction copper coin pipe is arranged 2 rows suitable for reading, adds the fire door material, beats and builds compacting, the formation fire door;
5) give induction copper coin pipe dispatch electricity, make fire door alcohol and possibly volatilize fully by remaining steam with 50 ~ 250 ℃ of baking 1.5h, again with 250 ~ 1650 ℃ of baking 8h, during baking, Open Side Down on induction copper coin pipe row top tilts 45 °;
6) the induction furnace Vakuumkammer that closes is evacuated to 50 ~ 80Pa earlier, and argon filling carries out the argon envelope again, with 1600 ℃ of sintering 1.5h;
7) take out the agglomerating crucible, adding the prepurging of steel material steel can accomplish;
Wherein, the weight percent content of each component is in the said crucible furnace building material: 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 quicklime 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%;
Said fire door material is to be that 98% magnesium oxide sand and weight ratio are that 2% boric acid powder mixes the back and adds the paste-like material that the industrial spirit modulation of purity 99% or more forms, all satisfied 0＜granularity of this magnesium oxide sand and boric acid powder≤1mm by weight ratio.
Effect: furnace drying time amounts to 11 hours in the preparation process, shortens 54%; The interior vacuum tightness of preceding 2 stove Vakuumkammers of furnace life can reach 0.8Pa, and the 3rd stove can begin to smelt ultra-clean steel, and shift to an earlier date 60% opportunity; Crucible life 82 stoves prolong 64%.
Embodiment 3
1) in the induction copper coin pipe row of induction furnace, behind laying one deck woven asbesto, 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) in induction copper coin pipe row, put into graphite tire core, and keep graphite tire core and both axis coincidings of induction copper coin pipe row;
3) add the brickwork material to the gap of graphite tire core periphery, successively beat and build compacting, form body of heater;
4) the body of heater height is beaten and is built when induction copper coin pipe is arranged 2 rows 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, make fire door alcohol and possibly volatilize fully by remaining steam with 50 ~ 250 ℃ of baking 2h, again with 250 ~ 1650 ℃ of baking 8h, Open Side Down on induction copper coin pipe row top during baking tilts 50 °;
6) the induction furnace Vakuumkammer that closes is evacuated to 67Pa earlier, and applying argon gas carries out the argon envelope again, with 1700 ℃ of sintering 2h;
7) take out the agglomerating crucible, adding the prepurging of steel material steel can accomplish;
Wherein, the weight percent content of each component is in the said crucible furnace building material: 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 quicklime 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%;
Said fire door material is to be that 98% magnesium oxide sand and weight ratio are that 2% boric acid powder mixes the back and adds the paste-like material that the industrial spirit modulation of purity 99% or more forms, all satisfied 0＜granularity of this magnesium oxide sand and boric acid powder≤1mm by weight ratio.
Effect: furnace drying time amounts to 12 hours, shortens 50%; The interior vacuum tightness of preceding 2 stove Vakuumkammers of furnace life can reach 0.9Pa, and the 3rd stove can begin to smelt ultra-clean steel, and shift to an earlier date 70% opportunity; Crucible life 78 stoves prolong 56%.
Embodiment 4
1) in the induction copper coin pipe row of induction furnace, behind laying one deck woven asbesto, 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) in induction copper coin pipe row, put into graphite tire core, and keep graphite tire core and both axis coincidings of induction copper coin pipe row;
3) add the brickwork material to the gap of graphite tire core periphery, successively beat and build compacting, form body of heater;
4) the body of heater height is beaten and is built when induction copper coin pipe is arranged 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, make fire door alcohol and possibly volatilize fully by remaining steam with 50 ~ 250 ℃ of baking 1.5h, again with 250 ~ 1650 ℃ of baking 7.5h, Open Side Down on induction copper coin pipe row top during baking tilts 60 °;
6) the induction furnace Vakuumkammer that closes is evacuated to 67Pa earlier, and argon filling carries out the argon envelope again, with 1750 ℃ of sintering 2h;
7) take out the agglomerating crucible, adding the prepurging of steel material steel can accomplish;
Wherein, the weight percent content of each component is in the said crucible furnace building material: 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 quicklime 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%;
Said fire door material is to be that 98.5% magnesium oxide sand and weight ratio are that 1.5% boric acid powder mixes the back and adds the paste-like material that the industrial spirit modulation of purity 99% or more forms, all satisfied 0＜granularity of this magnesium oxide sand and boric acid powder≤1mm by weight ratio.
Effect: furnace drying time amounts to 11 hours, shortens 54%; The interior vacuum tightness of preceding 2 stove Vakuumkammers of furnace life can reach 0.8Pa, and the 3rd stove can begin to smelt ultra-clean steel, and shift to an earlier date 60% opportunity; Crucible life 82 stoves prolong 64%.
Embodiment 5
1) in the induction copper coin pipe row of induction furnace, behind laying one deck woven asbesto, 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) in induction copper coin pipe row, put into graphite tire core, and keep graphite tire core and both axis coincidings of induction copper coin pipe row;
3) add the brickwork material to the gap of graphite tire core periphery, successively beat and build compacting, form body of heater;
4) the body of heater height is beaten and is built when induction copper coin pipe is arranged 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, make fire door alcohol and possibly volatilize fully by remaining steam with 50 ~ 250 ℃ of baking 2h, again with 250 ~ 1650 ℃ of baking 7h, Open Side Down on induction copper coin pipe row top during baking tilts 40 °;
6) the induction furnace Vakuumkammer that closes is evacuated to 67Pa earlier, and argon filling carries out the argon envelope again, with 1750 ℃ of sintering 1.5h;
7) take out the agglomerating crucible, adding the prepurging of steel material steel can accomplish;
Wherein, in the said 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 quicklime 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%;
Said fire door material is to be that 97% magnesium oxide sand and weight ratio are that 3% boric acid powder mixes the back and adds the paste-like material that the industrial spirit modulation of purity 99% or more forms, all satisfied 0＜granularity of this magnesium oxide sand and boric acid powder≤1mm by weight ratio.
Effect: furnace drying time amounts to 10.5 hours, shortens 56%; The interior vacuum tightness of preceding 2 stove Vakuumkammers of furnace life can reach 0.75Pa, and the 3rd stove can begin to smelt ultra-clean steel, and shift to an earlier date 60% opportunity; Crucible life 79 stoves prolong 58%.
Claims (5)
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 may further comprise the steps successively:
1) in the induction copper coin pipe row of induction furnace, behind laying one deck priming material, in induction copper coin pipe row, adds the crucible furnace building material, beat and build compacting formation furnace bottom;
2) in induction copper coin pipe row, put into graphite tire core, and keep graphite tire core and the axis coinciding of responding to copper coin pipe row;
3) add the brickwork material to the gap of graphite tire core periphery, successively beat and build compacting, form body of heater;
4) the body of heater height is beaten and is built when induction copper coin pipe is arranged 1 ~ 2 row suitable for reading, adds the fire door material, beats and builds compacting, the formation fire door;
5) give induction copper coin pipe dispatch electricity, with 50 ~ 250 ℃ of baking 1 ~ 2h, again with 250 ~ 1650 ℃ of baking 6 ~ 8h;
6) the induction furnace Vakuumkammer that closes is evacuated to 50 ~ 80Pa earlier, and applying argon gas carries out the argon envelope again, with 1600 ~ 1750 ℃ of sintering 1 ~ 2h;
7) adding the prepurging of steel material steel can accomplish;
Wherein, the weight percent content of each component is in the said crucible furnace building material: 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 quicklime 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%;
Said fire door material is that the boric acid powder by 95 ~ 98% magnesium oxide sand and 2 ~ 5% mixes the back and adds the paste-like material that the industrial spirit modulation of purity 99% or more forms, all satisfied 0＜granularity of said magnesium oxide sand and boric acid powder≤1mm by weight percentage.
2. according to the dry type making method of the said vacuum induction furnace of claim 1 from the magnesia crucible of sintering oxidation, it is characterized in that: in the said step 1), priming material is woven asbesto or glasscloth.
According to claim 1 or 2 said vacuum induction furnaces from the dry type making method of the magnesia crucible of sintering oxidation, it is characterized in that: said step 2), beating brickwork base thickness degree is 5 ~ 50mm.
According to claim 1 or 2 said vacuum induction furnaces from the dry type making method of the magnesia crucible of sintering oxidation, it is characterized in that: in the said step 5), Open Side Down on induction copper coin pipe row top during baking tilts 30 ~ 60 °.
5. according to the dry type making method of the said vacuum induction furnace of claim 3 from the magnesia crucible of sintering oxidation, it is characterized in that: in the said step 5), Open Side Down on induction copper coin pipe row top during baking tilts 30 ~ 60 °.
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| CN108218414A (en) * | 2016-12-21 | 2018-06-29 | 中国科学院金属研究所 | A kind of preparation method of high-capacity vacuum sensing smelting combined oxidation calcium 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 |
| CN112430783A (en) * | 2020-10-29 | 2021-03-02 | 钢铁研究总院 | Nickel-saving type air valve alloy and preparation method thereof |
| CN112321282A (en) * | 2020-11-05 | 2021-02-05 | 山东瑞泰新材料科技有限公司 | High-strength magnesium oxide crucible and preparation method thereof |
| CN114410994A (en) * | 2021-12-30 | 2022-04-29 | 北京科技大学 | Based on CaO-MgO-Al2O3Method for smelting nickel-based high-temperature alloy by using refractory material |
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| CN115231916A (en) * | 2022-07-13 | 2022-10-25 | 西安西工大思强科技股份有限公司 | Magnesium aluminate spinel forming crucible and manufacturing method thereof |
| 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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