CN107857272A - A kind of method of ferrosilicon or metalluragical silicon dephosphorization - Google Patents
A kind of method of ferrosilicon or metalluragical silicon dephosphorization Download PDFInfo
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- CN107857272A CN107857272A CN201710878510.2A CN201710878510A CN107857272A CN 107857272 A CN107857272 A CN 107857272A CN 201710878510 A CN201710878510 A CN 201710878510A CN 107857272 A CN107857272 A CN 107857272A
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- Prior art keywords
- ferrosilicon
- dephosphorization
- silicon
- hydrogen
- metalluragical silicon
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 229910000519 Ferrosilicon Inorganic materials 0.000 title claims abstract description 48
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 41
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000010703 silicon Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000007789 gas Substances 0.000 claims abstract description 35
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052786 argon Inorganic materials 0.000 claims abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 21
- 229910052698 phosphorus Inorganic materials 0.000 claims description 21
- 239000011574 phosphorus Substances 0.000 claims description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 239000008246 gaseous mixture Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000007670 refining Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 230000005672 electromagnetic field Effects 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 5
- 238000000746 purification Methods 0.000 description 4
- 238000005272 metallurgy Methods 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000007173 Abies balsamea Nutrition 0.000 description 1
- 241000723367 Conium maculatum Species 0.000 description 1
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 241000720974 Protium Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229920004482 WACKER® Polymers 0.000 description 1
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- VJTAZCKMHINUKO-UHFFFAOYSA-M chloro(2-methoxyethyl)mercury Chemical compound [Cl-].COCC[Hg+] VJTAZCKMHINUKO-UHFFFAOYSA-M 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/04—Removing impurities by adding a treating agent
- C21C7/064—Dephosphorising; Desulfurising
Abstract
The present invention relates to a kind of method of ferrosilicon or metalluragical silicon dephosphorization, belongs to refining techniques field.Under vacuum, ferrosilicon or metalluragical silicon are placed in floatation device first and are preheating to 1300 ~ 2500 DEG C of formation molten drops；It is passed through hydrogen argon gas mixed gas simultaneously, control input electric current is 300 ~ 400A, frequency is 150kHz ~ 400kHz and input power range is 3000 ~ 4500W, molten drop is suspended 5 ~ 40 minutes, each suspension time interval at least 5 minutes, obtains dephosphorization ferrosilicon or metalluragical silicon.This method makes the P elements in Antaciron be reduced to a lower standard, and without the secondary pollution of sidewall of crucible, specifically make specimen suspension under electromagnetic field effect, while use hydrogen argon gas mixed gas, so as to be had great significance in reduction production cost and raising efficiency etc..
Description
Technical field
The present invention relates to a kind of method of ferrosilicon or metalluragical silicon dephosphorization, belongs to refining techniques field.
Background technology
Solar energy receives much concern in recent years as a kind of important clean energy resource.In order to rationally utilize this cleaning
The energy, world's photovoltaic industry quickly flourish, and correlation technique obtains the extensive concern of industrial quarters.However, high-purity low cost
Shortage of raw materials seriously constrain the development of this clean energy resource.Solar level is produced using cheap metallurgical industry silicon
Silicon materials, the novel production process of high efficiency, low cost is developed, be a kind of economic means of the solar cell of production low cost.
Requirement of the solar energy level silicon to impurity content is very strict, it is desired to which purity reaches or close to 6N.At present, solar level
The production technology of polysilicon is mainly improved Siemens and silane decomposition, is referred to as chemical method, and chemical method prepares the sun
Energy level polycrystalline silicon technology is controlled and monopolized by developed countries such as the U.S., Germany, Japan, accounts for the 95% of Gross World Product, main more
There are Dow Coming (including Hemlock), SGS and a MEMC in the U.S. in crystal silicon manufacturing enterprise, Japanese Tokuyama, JFE,
Mitsubishi, Sumitomo and NS Solar Material, German Wacker, the ElkemSolar of Norway and China
STP etc..
Either traditional silane thermal decomposition process and Siemens Method solar level crystalline silicon production technology, or based on both approaches
The technique of improvement, there is the shortcomings that same：Cost is high, the construction period is long, investment is big, pollution weight, and key technology is external
Fewer companies monopolize.This aspect limits the further genralrlization of the technology.So metallurgy method purification prepares solar energy level silicon is
Current study hotspot.Metallurgy method mainly using the Methods For Purification metallurgical grade silicon of melt refining, mainly includes：Wet-process refining, electricity
Beamlet smelting process, plasma refining, directional solidification, slag practice, the methods of vacuum melting method.
Either traditional method or metallurgy method, the removing of phosphorus also become the main of solar energy level silicon production process and ground
Study carefully object.Although industry has trial more to this, economic and environment-friendly flow is not developed yet.Therefore, exploitation can be from silicon effectively
Deviate from the new technique of phosphorus, be the solar energy that raising that people have been working hard seek not only energy-conserving and environment-protective but also easily realized is produced
The quality technology of level silicon.
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of side of ferrosilicon or metalluragical silicon dephosphorization
Method.This method makes the P elements in Antaciron be reduced to a lower standard, and without the secondary pollution of sidewall of crucible, specifically
It is to make specimen suspension under electromagnetic field effect, while uses hydrogen-argon mixed gas, so as to is reducing production cost and raising
Efficiency etc. has great significance.The present invention is achieved through the following technical solutions.
A kind of method of ferrosilicon or metalluragical silicon dephosphorization, it is comprised the following steps that：First by Antaciron or metalluragical silicon
Sample is cut into sheet, is 0.58 ~ 0.65g with electronic scale ferrosilicon ferrosilicon or metalluragical silicon weight（±0.01）, then by ferrosilicon or
Metallurgical silicon sample is placed into the floater equipment of the water cooling copper coil of energization, and floater is sealed, pre- in floatation device
Heat 15 ~ 20 minutes, to 1300 ~ 2500 DEG C of formation molten drops, while the hydrogen-argon mixed gas after purification is passed through, uses gaseous mixture
Body purges the device 1 ~ 2 minute, and control input electric current is 300 ~ 400A, frequency is 150kHz ~ 400kHz and input power model
Enclose for 3000 ~ 4500W, molten drop is suspended 5 ~ 40 minutes, suspend 3 ~ 8 times, at least every 5 minutes between each suspension time, taken off
Phosphorus ferrosilicon or metalluragical silicon.
The Silicon in Ferrosilicon content is 65 ~ 85wt%, and phosphorus content is 0.0060 ~ 0.0500wt%.
Silicone content is 98 ~ 99wt% in the metalluragical silicon, and phosphorus content is 0.0020 ~ 0.0050wt%.
Hydrogen volume content is 0% to 100% in the hydrogen-argon mixed gas, the stream of hydrogen-argon mixed gas
Measure as 0.25 ~ 1.2L/min.
Inventive principle of the present invention：
In adjustment input current and in the case that frequency causes power in OK range, magnetic field size inside Serpentine Gallery Pavilion and
Distribution situation can meet the floating condition of the Antaciron of certain mass.After Antaciron sample is successfully suspended refining,
P elements in Antaciron can be removed effectively.Reaction equation using hydrogen-argon mixed gas dephosphorization is shown in formula 1.
2[P]Fe(wt%, H dissolve in Fe)=P2(g) （Formula 1）
Analysis understands that in suspension refining process, the protium in gas system can dissolve in Antaciron and react,
Help to remove the phosphorus impurities in molten metal.The hydrogen dissolved in is believed to cause the resistance and evaporation of P elements in Antaciron
Effect, cause good dephosphorization dynamic conditions.
The beneficial effects of the invention are as follows：
（1）During using hydrogen-argon mixed gas dephosphorization, phosphorus content can remove 40% of mass percent or so.
（2）The caused recyclable storage of phosphorus gas utilizes, free from environmental pollution.
（3）Dephosphorization is carried out to ferrosilicon or metallurgical silicon sample using this method, ferrosilicon or metallurgical silicon sample after dephosphorization
Middle phosphorus content is only 0.0338~0.000022wt%.
Brief description of the drawings
Fig. 1 is the dephosphorization effect figure of the embodiment of the present invention 1.
Embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
The method of the ferrosilicon or metalluragical silicon dephosphorization, it is comprised the following steps that：First by 0.65g ferrosilicon（15%Fe-85%Si is closed
Gold, phosphorus content 0.0500wt%）Ferrosilicon sample is placed into the floater equipment of water cooling copper coil of energization again, and will be outstanding
Floating chamber seals.It is placed in floatation device and preheats 15 minutes, to 1360 DEG C of formation molten drop.The hydrogen-argon being passed through simultaneously after purification
Mixed gas, purge the device 1 ~ 2 minute with mixed gas, hydrogen volume content is 0%H in hydrogen-argon mixed gas2, hydrogen
The flow of gas-argon gas mixed gas is 0.25L/min.Control input electric current is 300A, frequency is 150kHz and input power
Scope is 3000W, molten drop is suspended respectively 5,10,20,40 minutes, suspends 4 times, 5 minute minute of suspension time interval, is taken off
Phosphorus ferrosilicon.
The design sketch of dephosphorization ferrosilicon is as shown in figure 1, as seen from Figure 1, increase over time, phosphorus content becomes in reduction
Gesture dephosphorization effect very significantly, was almost stripped of 40% of phosphorus content in Antaciron in first 20 minutes, but after 20 minutes,
Phosphorus content can not almost reduce again.
Embodiment 2
The method of the ferrosilicon or metalluragical silicon dephosphorization, it is comprised the following steps that：First by 0.59g ferrosilicon（65wt%Si-35wt%Fe
Alloy, phosphorus content 0.0427wt%）, then ferrosilicon sample is placed into the floater equipment of water cooling copper coil of energization, and will
Floater seals.It is placed in floatation device and preheats 20 minutes, to 2000 DEG C of formation molten drop；It is passed through hydrogen-argon gaseous mixture simultaneously
Body, hydrogen volume content is 5%H in hydrogen-argon mixed gas2, the flow of hydrogen-argon mixed gas is 0.45L/min,
The device is purged with mixed gas 1 minute.Control input electric current is 320A, frequency is 180kHz and input power range is
3200W, molten drop is suspended 5 minutes, suspended 3 times, be 10 minutes between each suspension time, obtain dephosphorization ferrosilicon.
Phosphorous 0.0338wt% in the dephosphorization ferrosilicon.
Embodiment 3
The method of the ferrosilicon or metalluragical silicon dephosphorization, it is comprised the following steps that：First by 0.59g ferrosilicon（70wt%Si-30wt%Fe
Alloy, phosphorus content 0.0060wt%）, then ferrosilicon sample is placed into the floater equipment of water cooling copper coil of energization, and will
Floater seals.It is placed in floatation device and preheats 20 minutes, to 1800 DEG C of formation molten drop；It is passed through hydrogen-argon gaseous mixture simultaneously
Body, hydrogen volume content is 25%H in hydrogen-argon mixed gas2, the flow of hydrogen-argon mixed gas is 1.2L/min,
The device is purged with mixed gas 1.5 minutes, and control input electric current is 400A, frequency is 400kHz and input power range is
4500W, molten drop is suspended 20 minutes, suspend 3 times, at least every 5 minutes between each suspension time, obtain dephosphorization ferrosilicon.
Phosphorous 0.00362wt% in the dephosphorization ferrosilicon.
Embodiment 4
The method of the ferrosilicon or metalluragical silicon dephosphorization, it is comprised the following steps that：First by 0.58g ferrosilicon（75wt%Si-25wt%Fe
Alloy, phosphorus content 0.0260wt%）, then ferrosilicon sample is placed into the floater equipment of water cooling copper coil of energization, and will
Floater seals.It is placed in floatation device and preheats 18 minutes, to 1300 DEG C of formation molten drop；It is passed through hydrogen-argon gaseous mixture simultaneously
Body, hydrogen volume content is 50%H in hydrogen-argon mixed gas2, the flow of hydrogen-argon mixed gas is 1.00L/min,
The device is purged with mixed gas 2 minutes, and control input electric current is 340A, frequency is 200kHz and input power range is
3600W, molten drop is suspended 10 minutes, suspend 8 times, at least every 5 minutes between each suspension time, obtain dephosphorization ferrosilicon.
Phosphorous 0.0135wt% in the dephosphorization ferrosilicon.
Embodiment 5
The method of the ferrosilicon or metalluragical silicon dephosphorization, it is comprised the following steps that：First by 0.64g ferrosilicon（85wt%Si-15wt%Fe
Alloy, phosphorus content 0.0489wt%）Ferrosilicon sample is placed into the floater equipment of water cooling copper coil of energization again, and will
Floater seals.It is placed in floatation device and is preheating to 2500 DEG C of formation molten drops；While hydrogen-argon mixed gas is passed through, hydrogen-
Hydrogen volume content is 0%H in argon gas mixed gas2, the flow of hydrogen-argon mixed gas is 1.2L/min, uses mixed gas
Purge the device 2 minutes.Control input electric current is 400A, frequency is 400kHz and input power range is 4000W, by molten drop
Suspend 40 minutes, suspend 3 times, at least every 5 minutes between each suspension time, obtain dephosphorization ferrosilicon.
Phosphorous 0.0293wt% in the dephosphorization ferrosilicon.
Embodiment 6
The method of the ferrosilicon or metalluragical silicon dephosphorization, it is comprised the following steps that：First by 0.63g metalluragical silicons（Silicone content is
99wt%, phosphorus content 0.0050wt%）It is placed into the floater equipment of the water cooling copper coil of energization, and floater is sealed.
It is placed in floatation device and is preheating to 2400 DEG C of formation molten drops；It is passed through hydrogen-argon mixed gas, hydrogen-argon gaseous mixture simultaneously
Hydrogen volume content is 100%H in body2, the flow of hydrogen-argon mixed gas is 1.0L/min, and the dress is purged with mixed gas
Put 2 minutes.Control input electric current is 360A, frequency is 260kHz and input power range is 3800W, and molten drop is suspended 20 points
Clock, obtain dephosphorization metallurgical grade silicon.
Phosphorous 0.000022wt% in the dephosphorization metalluragical silicon.
Above in association with accompanying drawing to the present invention embodiment be explained in detail, but the present invention be not limited to it is above-mentioned
Embodiment, can also be before present inventive concept not be departed from those of ordinary skill in the art's possessed knowledge
Put that various changes can be made.
Claims (4)
1. a kind of method of ferrosilicon or metalluragical silicon dephosphorization, it is characterised in that comprise the following steps that：Under vacuum, first will
Ferrosilicon or metalluragical silicon, which are placed in floatation device, is preheating to 1300 ~ 2500 DEG C of formation molten drops；It is passed through hydrogen-argon gaseous mixture simultaneously
Body, control input electric current is 300 ~ 400A, frequency is 150kHz ~ 400kHz and input power range is 3000 ~ 4500W, will
Molten drop suspends 5 ~ 40 minutes, each suspension time interval at least 5 minutes, obtains dephosphorization ferrosilicon or metalluragical silicon.
2. the method for ferrosilicon according to claim 1 or metalluragical silicon dephosphorization, it is characterised in that：The Silicon in Ferrosilicon content
For 65 ~ 85wt%, phosphorus content is 0.0500 ~ 0.0060wt%.
3. the method for ferrosilicon according to claim 1 or metalluragical silicon dephosphorization, it is characterised in that：Silicon contains in the metalluragical silicon
It is 0.0020 ~ 0.0050wt% to measure as 98 ~ 99wt%, phosphorus content.
4. the method for ferrosilicon according to claim 1 or metalluragical silicon dephosphorization, it is characterised in that：The hydrogen-argon mixes
It is 0 to 100% to close hydrogen volume content in gas, and the flow of hydrogen-argon mixed gas is 0.25 ~ 1.2L/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710878510.2A CN107857272A (en) | 2017-09-26 | 2017-09-26 | A kind of method of ferrosilicon or metalluragical silicon dephosphorization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710878510.2A CN107857272A (en) | 2017-09-26 | 2017-09-26 | A kind of method of ferrosilicon or metalluragical silicon dephosphorization |
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| Publication Number | Publication Date |
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| CN107857272A true CN107857272A (en) | 2018-03-30 |
Family
ID=61699576
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710878510.2A Pending CN107857272A (en) | 2017-09-26 | 2017-09-26 | A kind of method of ferrosilicon or metalluragical silicon dephosphorization |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754072A (en) * | 2018-05-29 | 2018-11-06 | 昆明理工大学 | A kind of stainless steel dephosphorization method |
| CN113621869A (en) * | 2021-08-27 | 2021-11-09 | 昆明理工大学 | Method for removing silicon and phosphorus from iron-silicon-phosphorus alloy containing platinum group metal |
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| CN102398905A (en) * | 2010-09-14 | 2012-04-04 | 赵钧永 | Method and equipment for refining silicon and obtained silicon crystal |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108754072A (en) * | 2018-05-29 | 2018-11-06 | 昆明理工大学 | A kind of stainless steel dephosphorization method |
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Application publication date: 20180330 |