CN207347178U - A kind of device of silicon melt external refining - Google Patents
A kind of device of silicon melt external refining Download PDFInfo
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- CN207347178U CN207347178U CN201720788265.1U CN201720788265U CN207347178U CN 207347178 U CN207347178 U CN 207347178U CN 201720788265 U CN201720788265 U CN 201720788265U CN 207347178 U CN207347178 U CN 207347178U
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- silicon melt
- silicon
- maing ladle
- refining
- circle
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 118
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 239000010703 silicon Substances 0.000 title claims abstract description 114
- 238000007670 refining Methods 0.000 title claims abstract description 76
- 239000007921 spray Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 16
- 239000002893 slag Substances 0.000 abstract description 16
- 238000007664 blowing Methods 0.000 abstract description 9
- 239000000377 silicon dioxide Substances 0.000 abstract description 8
- 238000003723 Smelting Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 28
- 239000011575 calcium Substances 0.000 description 18
- 229910052791 calcium Inorganic materials 0.000 description 18
- 238000000034 method Methods 0.000 description 10
- 239000012535 impurity Substances 0.000 description 8
- 238000000746 purification Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 229920001296 polysiloxane Polymers 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 229910001634 calcium fluoride Inorganic materials 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 238000009423 ventilation Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002516 radical scavenger Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910000632 Alusil Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 150000001339 alkali metal compounds Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- -1 device A l Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
A kind of device of silicon melt external refining is the utility model is related to, belongs to purifying industrial silicon technology field.Bottom of two-maing ladle in the device sets two gas nozzles, and the angle theta of two nozzle centers of circle and bottom center of circle presentation of two-maing ladle meets:90°≤θ≤180°;Relation between the distance in two nozzle centers of circle and the bottom center of circle of two-maing ladle, spout radius r and the bottom radius R that two-mans ladle is:WhereinSet to bottom of two-maing ladle in two gas nozzles and be continually fed into compressed air or refinery gas, the silicon melt that mine heat furnace smelting goes out is put into in two-maing ladle, with the increase for interior release silicon melt of two-maing ladle, adds refining agent, and adjust and be passed through refinery gas component and flow, carry out air blowing, slag refining outside stove;Push the scum silica frost of silicon melt surface aside, carry out the cast of silicon melt, obtain high-purity industrial silicon product.The dynamic conditions of special interior silicon melt of two-maing ladle is ensure that in the utility model, is eliminated stirring dead angle, is effectively raised silicon product quality.
Description
Technical field
A kind of device of silicon melt external refining is the utility model is related to, belongs to purifying industrial silicon technology field.
Background technology
Industrial silicon industry is source and the basic industry of whole silicon industrial chain.Polysilicon and photovoltaic industry are to develop in recent years
Most fast, most promising industry.Industrial silicon industry and polysilicon and photovoltaic industry be belong to silicon industrial chain up and down
Product industry is swum, is restricted between quality and quantity close.China is the big producer of industrial silicon, China's industrial silicon yield in 2016
For 225.20 ten thousand tons, increase by 4.74% on a year-on-year basis.
Photovoltaic industry develops rapidly, and the demand of polysilicon solar cell is growing, alusil alloy, organosilicon compared with
Fast development, these all drive the fast development of industrial silicon, its market demand increase is also increasingly notable.Scientific and technological production development it is same
When, market is also higher and higher to the quality requirement of industrial silicon, and existing industrial silicon production technology gradually can not meet market will
Ask.Therefore, more impurity in industrial silicon how are removed, high-purity industrial silicon is prepared and is asked as what each production production man paid close attention to
Topic.In the industrial production, the most common impurity-removing method of industrial silicon plant is to carry out stove to the silicon melt that mineral hot furnace comes out in two-maing ladle
Outer refining.Zhang Anfu et al. (number of patent application:201110127717) bottom blowing compressed air and oxygen and additional refinements are passed through
Desulfurizing agent calcium stone, makes the aluminium accelerated oxidation in silicon liquid, forms oxidizing slag, effectively removes impurity A l contents, improve industrial silicon
Product quality.Jihong ZHOU et al. (number of patent application:201510654085) refined by first oxygen blast, then add certain proportion in due course
Magnesium salts and sodium salt be mixed into combination wadding agent, effectively by metallurgical grade silicon lifted to chemical grade silicon grade.As can be seen that blow
Refining and slag refining can effectively remove partial impurities in industrial silicon, improve silicon product quality.
In fact, the bottom of two-maing ladle used in the furnace outer refining technology of invention only has a nozzle.In actual production, one
The bottom blowing refining of a nozzle can both make silicon melt stir insufficient, uneven components in silicon melt, so as to influence product quality, again
Cause refining time longer, thermal loss is more, finally influences yield, increases energy consumption.Lifted using the twin-jet nozzle of rational position arrangement
Bag carries out external refining, can effectively solve the above problems in the case where excessively not increasing capital expenditure.
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the utility model provides a kind of dress of silicon melt external refining
Put.The device of the utility model strengthens external refining in refining using special two-man ladle of bottom twin-jet nozzle, and the utility model leads to
Cross following technical scheme realization.
A kind of device of silicon melt external refining, the bottom 2 of two-maing ladle set two gas nozzles 3, two 3 centers of circle of nozzle and
The angle theta that the bottom center of circle is presented of two-maing ladle meets:90°≤θ≤180°;The distance 1 in two 3 centers of circle of nozzle and the bottom center of circle of two-maing ladle,
Relation between 3 radius r of nozzle and the 2 radius R of bottom that two-mans ladle is:Wherein
A kind of application process of the device of silicon melt external refining, it is comprised the following steps that:
Step 1, set in two gas nozzles 3 to bottom 2 of two-maing ladle and be continually fed into compressed air or refinery gas, to two-maing ladle
In be put into the silicon melt that mine heat furnace smelting goes out, with two-man ladle it is interior release silicon melt increase, add refining agent, and adjust be passed through essence
Gas componant and flow are refined, carries out air blowing, slag refining outside stove;
After step 2, silicon melt external refining, the scum silica frost of silicon melt surface is pushed aside, after realizing the separation of slag silicon, carry out silicon
The cast of melt, obtains high-purity industrial silicon product.
It is 0.5~15m that the step 1, which is passed through refinery gas flow,3/ h, pressure are 1~15MPa, duration of ventilation for 0.3~
8h.Above-mentioned refinery gas includes but not limited to:One or more of gas arbitrary proportions in air, oxygen-enriched air, vapor etc.
Mixed gas.
The step 1 refining agent addition is 20 with silicon melt mass ratio:1~1:20.The feed postition of refining agent includes:
Disposable addition, in batches addition etc.;Refining agent refines general refining agent for silicon melt, includes but not limited to:CaO、CaF2、
SiO2, the Ith and II one or more refining agent arbitrary proportions in main group alkali metal compound etc. admixture refining agent.
The utility model aim to solve the problem that using it is existing two-man ladle carry out external refining when, interior silicon melt stirring of two-maing ladle is insufficient,
In the presence of stirring dead angle, cause to wrap interior melt quality uneven;Refining time is grown, and silicon melt thermal loss is more, so as to influence yield
Realistic problem.After the fully process characteristic and actual condition of research industrial silicon external refining, the utility model is directly right
Two-man ladle and transformed, by setting two nozzles in bottom appropriate location of two-maing ladle, the scavenger system of each self-configuring independence, is made
Slag, joint of blowing refining, utilize the heat of silicon melt, improve product quality, wherein Al, Ca, Ti, C impurity content well
Significantly reduce than before.
Method described in the utility model be using bottom twin-jet nozzle it is special two-man ladle blown, slag refining.Herein
During external refining, can according to special interior silicon melt amount of two-maing ladle number, the spraying state of silicon melt, rationally adjustment is each
Gas flow, gas pressure and the gas ingredients of nozzle so that it is special two-man ladle interior silicon melt without flowing " dead band ", realize refining when
Between shorter, refining process that refining efficiency is higher.This discovery is with refining effect is good, production efficiency is high, capital expenditure is few, environment
It is pollution-free, it is easy to the features such as heavy industrialization is applied.
The utility model has the advantage that:
(1) refining effect is good:The utility model twin-jet nozzle it is special two-man ladle in carry out external refining, ensure that special lift
The dynamic conditions of silicon melt in bag, eliminates stirring dead angle, effectively raises silicon product quality.
(2) production efficiency is high;External refining using the utility model it is special two-man ladle blown, slag refining, pass through
Gas flow, the gas pressure of each nozzle, two nozzle interruptions or the operation such as injection at the same time are adjusted, industrial silicon melt is realized
High efficiency purifies.
(3) capital expenditure is few;The utility model only need to carry out reasonable reformation to two-maing ladle, and the specific location in bottom of two-maing ladle is pacified
Two nozzles are filled, increase an independent scavenger system, equipment is simple, facilitates feasible.
(4) environmental nonpollution;It is small to environmental pressure since this process will not produce secondary pollution, therefore can realize green
It is metallurgical.
Brief description of the drawings
Fig. 1 is 1 structure drawing of device of the utility model embodiment;
Fig. 2 is the specific dimensional structure figure of 1 device of the utility model embodiment;
Fig. 3 is the specific dimensional structure figure of 2 device of the utility model embodiment;
Fig. 4 is the specific dimensional structure figure of 3 device of the utility model embodiment.
In figure:1- two-mans ladle mouth, and 2- two-mans ladle bottom, 3- nozzles.
Embodiment
With reference to the accompanying drawings and detailed description, the utility model is described in further detail.
Embodiment 1
As illustrated in fig. 1 and 2, the device of the silicon melt external refining, two gas nozzles 3 of the setting of bottom 2 of two-maing ladle, two
The angle theta of 3 center of circle of nozzle and bottom center of circle presentation of two-maing ladle (meets for 120 °:90°≤θ≤180°);Two 3 centers of circle of nozzle and lift
The distance 1 for wrapping the bottom center of circle is that 0.5R, 3 radius r of nozzle are 0.2R, is metWherein
The application process of the device of the silicon melt external refining, it is comprised the following steps that:
Step 1, set to bottom 2 of two-maing ladle and compressed air be continually fed into two gas nozzles 3 (flow of compressed air is
8m3/ h), silicon melt that mine heat furnace smelting goes out is put into in two-maing ladle (mainly including following mass percent component:96%Si,
0.8%Al, 3%Ca), with the increase for interior release silicon melt of two-maing ladle, it is 10 to add mass ratio:1:10 SiO2、CaF2With
Al2O3(refining agent addition is 20 with silicon melt mass ratio to refining agent:1), and by two gas nozzles 3 logical oxygen-enriched air (oxygen is changed
Gas is 9 with volume of air ratio:1, the oxygen-enriched air pressure being passed through is 5MPa, flow 10m3/ h), carry out air blowing, slag making outside stove
Refine 0.3h (i.e. duration of ventilation is 0.3h);
After step 2, silicon melt external refining, the scum silica frost of silicon melt surface is pushed aside, after realizing the separation of slag silicon, carry out silicon
The cast of melt, obtains high-purity industrial silicon product.
Al content in the industrial silicon product that the present embodiment is prepared<0.1wt%, Ca content<0.02wt%, silicone content are
99.6%.The equipment (nozzle 1 only is set in bottom centre position of two-maing ladle) of existing conventional silicon melt external refining purification with
Al content in the silicon product being prepared under the identical Parameter Conditions of the present embodiment<0.3wt%, Ca content<0.04wt%, silicon contain
Measure as 99.3%, hence it is evident that it can be seen that the impurity such as device A l, Ca, Ti, C of industrial silicon melt external refining purification of the application contains
Amount is efficiently removed, and improves refining effect.
Embodiment 2
As shown in figure 3, the device of the silicon melt external refining, the bottom 2 of two-maing ladle sets two gas nozzles 3, two sprays
The angle theta of 3 center of circle of mouth and bottom center of circle presentation of two-maing ladle (meets for 90 °:90°≤θ≤180°);Two 3 centers of circle of nozzle are with two-maing ladle
The distance 1 in the bottom center of circle is that 0.3R, 3 radius r of nozzle are 0.2R, is metWherein
The application process of the device of the silicon melt external refining, it is comprised the following steps that:
Step 1, set to bottom 2 of two-maing ladle and compressed air be continually fed into two gas nozzles 3 (flow of compressed air is
8m3/ h), silicon melt that mine heat furnace smelting goes out is put into in two-maing ladle (mainly including following mass percent component:96%Si,
0.8%Al, 3%Ca), with the increase for interior release silicon melt of two-maing ladle, it is 10 to add mass ratio:1:2 NaO, CaF2And Al2O3
(refining agent addition is 1 with silicon melt mass ratio to refining agent:20), and by two gas nozzles 3 the water flowing steam (water being passed through is changed
Steam pressure is 15MPa, flow 0.5m3/ h), carry out air blowing, slag refining 2h outside stove (i.e. duration of ventilation is 2h);
After step 2, silicon melt external refining, the scum silica frost of silicon melt surface is pushed aside, after realizing the separation of slag silicon, carry out silicon
The cast of melt, obtains high-purity industrial silicon product.
Al content in the industrial silicon product that the present embodiment is prepared<0.1wt%, Ca content<0.01wt%, B<10ppm,
Silicone content is 99.6%.The equipment of existing conventional silicon melt external refining purification (only sets spray in bottom centre position of two-maing ladle
Mouth 1) Al content in the silicon product that is prepared under the Parameter Conditions identical with the present embodiment<0.2wt%, Ca content<
0.04wt%, silicone content 99.3%, hence it is evident that it can be seen that the device A l of the industrial silicon melt external refining purification of the application,
The impurity contents such as Ca, Ti, C are efficiently removed, and improve refining effect.
Embodiment 3
As shown in figure 4, the device of the silicon melt external refining, the bottom 2 of two-maing ladle sets two gas nozzles 3, two sprays
The angle theta of 3 center of circle of mouth and bottom center of circle presentation of two-maing ladle (meets for 180 °:90°≤θ≤180°);Two 3 centers of circle of nozzle are with two-maing ladle
The distance 1 in the bottom center of circle is that 0.7R, 3 radius r of nozzle are 0.2R, is metWherein
The application process of the device of the silicon melt external refining, it is comprised the following steps that:
Step 1, set to bottom 2 of two-maing ladle and compressed air be continually fed into two gas nozzles 3 (flow of compressed air is
12m3/ h), silicon melt that mine heat furnace smelting goes out is put into in two-maing ladle (mainly including following mass percent component:96%Si,
0.8%Al, 3%Ca), with the increase for interior release silicon melt of two-maing ladle, addition mass ratio is CaO:MgO:CaF2=6:3:1 refining
(refining agent addition is 10 with silicon melt mass ratio for agent:1), and by two gas nozzles 3 logical volume ratio is changed as 1:1 hydrogen and
(mixture pressure being passed through is 1MPa, flow 15m to nitrogen mixed gas3/ h), carry out air blowing, slag refining 8h outside stove
(i.e. duration of ventilation is 8h);
After step 2, silicon melt external refining, the scum silica frost of silicon melt surface is pushed aside, after realizing the separation of slag silicon, carry out silicon
The cast of melt, obtains high-purity industrial silicon product.
Al content in the industrial silicon product that the present embodiment is prepared<0.08wt%, Ca content<0.005wt%, B<
8ppm, silicone content 99.7%.The equipment of existing conventional silicon melt external refining purification (is only installed in bottom interposition of two-maing ladle
Put nozzle 1) Al content in the silicon product that is prepared under the Parameter Conditions identical with the present embodiment<0.2wt%, Ca content<
0.02wt%, silicone content 99.4%, hence it is evident that it can be seen that the device A l of the industrial silicon melt external refining purification of the application,
The impurity contents such as Ca, Ti, C are efficiently removed, and improve refining effect.
Embodiment 4
The device of the silicon melt external refining, the bottom 2 of two-maing ladle set two gas nozzles 3, two 3 centers of circle of nozzle and lift
The angle theta that the bottom center of circle is presented is wrapped for 150 ° (to meet:90°≤θ≤180°);Two 3 centers of circle of nozzle and the bottom center of circle of two-maing ladle
Distance 1 is3 radius r of nozzle isMeetWherein
The application process of the device of the silicon melt external refining, it is comprised the following steps that:
Step 1, set to bottom 2 of two-maing ladle and compressed air be continually fed into two gas nozzles 3 (flow of compressed air is
15m3/ h unit), silicon melt that mine heat furnace smelting goes out is put into in two-maing ladle (mainly including following mass percent component:96%
Si, 0.8%Al, 3%Ca), with the increase for interior release silicon melt of two-maing ladle, add CaO:MgO:CaF2=6:3:1 refining agent (essence
It is 1 that agent addition, which is refined, with silicon melt mass ratio:10), and by two gas nozzles 3 logical volume ratio is changed as 1:1:1 hydrogen gas and water is steamed
(mixture pressure being passed through is 5MPa, flow 10m for vapour and nitrogen mixed gas3/ h), carry out air blowing, slag refining outside stove
2h (i.e. duration of ventilation is 2h);
After step 2, silicon melt external refining, the scum silica frost of silicon melt surface is pushed aside, after realizing the separation of slag silicon, carry out silicon
The cast of melt, obtains high-purity industrial silicon product.
Al content in the industrial silicon product that the present embodiment is prepared<0.06wt%, Ca content<0.005wt%, B<
8ppm, silicone content 99.7%.The equipment of existing conventional silicon melt external refining purification (is only installed in bottom interposition of two-maing ladle
Put nozzle 1) Al content in the silicon product that is prepared under the Parameter Conditions identical with the present embodiment<0.2wt%, Ca content<
0.015wt%, silicone content 99.5%, hence it is evident that it can be seen that the device A l of the industrial silicon melt external refining purification of the application,
The impurity contents such as Ca, Ti, C are efficiently removed, and improve refining effect.
Specific embodiment of the present utility model is explained in detail above in association with attached drawing, but the utility model is not
It is limited to the above embodiment, within the knowledge of a person skilled in the art, this practicality can also be not being departed from
Various changes can be made on the premise of new objective.
Claims (1)
- A kind of 1. device of silicon melt external refining, it is characterised in that:Two-man ladle bottom (2) set two gas nozzles (3), two spray The angle theta of mouth (3) center of circle and bottom center of circle presentation of two-maing ladle meets:90°≤θ≤180°;Two nozzle (3) centers of circle and bottom of two-maing ladle Relation between the distance 1 in the center of circle, nozzle (3) radius r and bottom of two-maing ladle (2) radius R is:Wherein
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107352546A (en) * | 2017-06-30 | 2017-11-17 | 昆明理工大学 | A kind of devices and methods therefor of silicon melt external refining |
CN113661258A (en) * | 2019-04-05 | 2021-11-16 | 杰富意钢铁株式会社 | Vessel for refining high temperature melt |
-
2017
- 2017-06-30 CN CN201720788265.1U patent/CN207347178U/en active Active
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107352546A (en) * | 2017-06-30 | 2017-11-17 | 昆明理工大学 | A kind of devices and methods therefor of silicon melt external refining |
CN113661258A (en) * | 2019-04-05 | 2021-11-16 | 杰富意钢铁株式会社 | Vessel for refining high temperature melt |
US11976340B2 (en) | 2019-04-05 | 2024-05-07 | Jfe Steel Corporation | Refining vessel for high-temperature melt |
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