CN112430756A - Niobium-iron alloy production method - Google Patents
Niobium-iron alloy production method Download PDFInfo
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- CN112430756A CN112430756A CN202011092014.2A CN202011092014A CN112430756A CN 112430756 A CN112430756 A CN 112430756A CN 202011092014 A CN202011092014 A CN 202011092014A CN 112430756 A CN112430756 A CN 112430756A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- JMAHHHVEVBOCPE-UHFFFAOYSA-N [Fe].[Nb] Chemical compound [Fe].[Nb] JMAHHHVEVBOCPE-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910000640 Fe alloy Inorganic materials 0.000 title claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 97
- 239000002893 slag Substances 0.000 claims abstract description 69
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 54
- 239000000956 alloy Substances 0.000 claims abstract description 54
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 25
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 23
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910000592 Ferroniobium Inorganic materials 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000007670 refining Methods 0.000 claims abstract description 17
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 15
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 15
- 239000004571 lime Substances 0.000 claims abstract description 15
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims abstract description 13
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000010436 fluorite Substances 0.000 claims abstract description 13
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 13
- 238000010891 electric arc Methods 0.000 claims abstract description 11
- 238000007664 blowing Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- 239000010955 niobium Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 6
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- 238000003780 insertion Methods 0.000 claims description 2
- 230000037431 insertion Effects 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 abstract description 2
- 229910052758 niobium Inorganic materials 0.000 description 11
- 239000000463 material Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000003832 thermite Substances 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 229910000922 High-strength low-alloy steel Inorganic materials 0.000 description 1
- 238000007133 aluminothermic reaction Methods 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- ZFGFKQDDQUAJQP-UHFFFAOYSA-N iron niobium Chemical compound [Fe].[Fe].[Nb] ZFGFKQDDQUAJQP-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C35/00—Master alloys for iron or steel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a niobium-iron alloy production method, which comprises the steps of producing niobium-iron and refining the niobium-iron by an aluminothermic process; in the step of producing the ferrocolumbium by the aluminothermic method, the metallurgical grade niobium oxide: aluminum powder: iron oxide powder: lime: fluorite powder: mixing the saltpeter according to a proportion; putting the raw materials into a reactor, and igniting for reaction to obtain a ferrocolumbium alloy liquid, wherein the upper layer of the alloy liquid is a slag liquid layer; the refining steps are as follows: placing an electrode downwards into the slag liquid layer, and heating the slag liquid layer through an electric arc to ensure that the slag liquid layer keeps fluidity; blowing aluminum powder into the slag liquid to promote the aluminum powder to reduce the niobium element in the slag liquid out and enter the alloy liquid; the invention has the advantages of low energy consumption, simple process, short production period and no environmental pollution by using the thermit method and the electric arc heating aluminum spraying.
Description
Technical Field
The invention relates to the technical field of alloy production, in particular to a niobium-iron alloy production method.
Background
Ferrocolumbium is mainly used for smelting high-temperature (heat-resistant) alloys, stainless steel and high-strength low-alloy steel. The steel structure is refined, the strength, toughness and creep property of the steel can be improved, and the corrosion resistance of the steel is improved. Can play a role in refining the structure, so that the steel has good formability and welding performance. Niobium plays a role in solid solution strengthening and carbide precipitation strengthening in the high-temperature alloy, and the yield strength and the surface stability of the high-temperature alloy are improved. Niobium is a lighter weight of the refractory metals and is one of the factors that are heavily used in superalloys.
At present, the domestic production method for producing the niobium-iron alloy is niobium oxide thermite production, and international Brazilian niobium-iron is niobium concentrate electrothermal production.
The aluminothermic process uses aluminium as reducing agent, mixes aluminium, niobium oxide, iron oxide powder, slag-forming agent and heat-generating agent, etc. and charges them into furnace, and makes them produce direct ignition reaction to obtain the niobium-iron alloy, and its yield is low, only is about 94%.
The electroheating method for producing the niobium concentrate adopts an ore furnace, the period is long, the continuous operation is realized, and the alloy quality can not reach the national 60A standard.
Disclosure of Invention
It is necessary to provide a niobium-iron alloy production method, which comprises the steps of producing niobium-iron by an aluminothermic process and refining the niobium-iron;
the aluminothermic method for producing the ferrocolumbium comprises the following steps:
s11: mixing the following raw materials in parts by weight:
metallurgical grade niobium oxide: aluminum powder: iron oxide powder: lime: fluorite powder: saltpeter = 1: 0.45-0.7: 0.3-0.7: 0.05-0.15: 0.06-0.2: 0.01-0.05;
s12: carrying out ball milling and particle size screening on lime in the raw materials, and controlling the particle size to be not more than 3 mm; drying the aluminum powder, the fluorite powder and the saltpeter respectively to remove water;
s13: putting the raw materials into a reactor, and igniting for reaction to obtain a ferrocolumbium alloy liquid, wherein the upper layer of the alloy liquid is a slag liquid layer;
the refining steps are as follows:
s21: placing an electrode downwards into the slag liquid layer, and heating the slag liquid layer through an electric arc to ensure that the slag liquid layer keeps fluidity;
s22: and blowing aluminum powder into the slag liquid to promote the aluminum powder to reduce the niobium element in the slag liquid out and enter the alloy liquid.
The two steps of the invention comprise the steps of preparing the ferrocolumbium alloy by an aluminothermic method and adding the aluminum lean slag by electric arc heating and refining. The invention has the advantages of low energy consumption, simple process, short production period and no environmental pollution by using the thermit method and the electric arc heating aluminum spraying.
Detailed Description
The embodiment of the invention provides a niobium-iron alloy production method, which comprises the steps of producing niobium-iron by an aluminothermic process and refining the niobium-iron;
the aluminothermic method for producing the ferrocolumbium comprises the following steps:
s11: mixing the following raw materials in parts by weight (kilogram):
metallurgical grade niobium oxide: aluminum powder: iron oxide powder: lime: fluorite powder: saltpeter = 1: 0.45-0.7: 0.3-0.7: 0.05-0.15: 0.06-0.2: 0.01-0.05;
s12: carrying out ball milling and particle size screening on lime in the raw materials, and controlling the particle size to be not more than 3 mm; drying the aluminum powder, the fluorite powder and the saltpeter respectively to remove water;
s13: putting the raw materials into a reactor, and igniting for reaction to obtain a ferrocolumbium alloy liquid, wherein the upper layer of the alloy liquid is a slag liquid layer;
the refining steps are as follows:
s21: placing an electrode downwards into the slag liquid layer, and heating the slag liquid layer through an electric arc to ensure that the slag liquid layer keeps fluidity;
s22: blowing aluminum powder into the slag liquid to promote the aluminum powder to reduce the niobium element in the slag liquid out and enter the alloy liquid;
the chemical reactions involved in the steps of the invention are:
3Nb2O5+10Al=6Nb+5Al2O3
3Fe3O4+ 8Al=9Fe +4Al2O3
in the invention, in the alloy liquid obtained after the thermite violent reaction, the reaction yield of the niobium oxide reaches 94 percent at most, and 6 percent of niobium oxide still does not participate in the reaction and remains in the slag liquid. After the aluminothermic reaction, the temperature of the alloy liquid and the slag liquid layer is about more than 1500 ℃, the temperature of the slag liquid is higher and still in a liquid state, at the moment, electrodes are immediately introduced into the furnace, the slag layer is heated by electric arc, the heat in the slag liquid is fully utilized, the slag liquid is kept in an active state, aluminum powder is simultaneously sprayed, the aluminum powder and niobium oxide in the slag liquid are subjected to reduction reaction, niobium is displaced, and the specific gravity of the niobium is greater than that of the slag liquid, so the niobium naturally sinks into the alloy liquid, the niobium in the slag liquid is further purified, the niobium content in the alloy liquid is increased, and the yield of raw material reaction is increased.
In the prior art, the ferro-niobium alloy is produced by a thermite method alone, after alloy liquid is obtained, slag liquid is removed and discharged to be used as waste for treatment, niobium in the slag liquid cannot be extracted and used, and the yield of the alloy liquid is low. Because 90% of the slag liquid layer is oxides such as calcium oxide, aluminum oxide and the like, and the slag liquid layer is poor in conductivity and even non-conductive, in the prior art, the residual niobium element cannot be secondarily refined by an electric arc refining or high-temperature smelting mode after the slag liquid is pulled out and cooled. The scheme combines the aluminothermic process and the refining process skillfully, utilizes the characteristics of liquid state and high temperature of the slag liquid, can electrify and arc the electrode in a short time, and can quickly heat the slag layer because the resistance of the slag layer is large and the heating is quick, thereby promoting the reaction of the aluminum powder and residual niobium oxide in the slag liquid.
This is different from the prior art methods of preparing ferrocolumbium by using the thermite method alone and preparing ferrocolumbium by using the refining method alone. The single aluminothermic method is adopted to obtain the steps S11-S13 of the invention, the yield of the prepared ferrocolumbium alloy is only 94%, the single refining method is to directly refine cold raw materials by an electric arc furnace, the cold materials are required to be heated to a molten state through electric arc, and then heated to a high temperature for reaction, the reaction period of the process is long, the energy consumption is extremely high, the operability in actual production is low, and the precedent of directly adopting the refining method to produce the ferrocolumbium alloy is absent temporarily.
Further, in step S13, after the internal flame of the reactor disappears and the alloy liquid becomes stable, an electrode is inserted into the alloy liquid, and the refining reaction is conducted.
Furthermore, the insertion depth of the end part of the electrode is in contact with the surface of the alloy liquid, and the electrode is kept to be adjusted up and down within a small range after the current is stabilized.
Further, when the electrode is placed downwards, the current is observed, when the current is instantly increased to the range of 7900 +/-100A, the electrode is kept adjusted within the range of 2-10cm above the existing height, and the current is kept stable.
Further, in step S21, the electrode energization parameters are: voltage: 140V, current: 7900A, energization time: and 5-25 minutes, wherein the ratio of the amount of the injected aluminum powder to the amount of the niobium oxide in the slag is 1: 0.005-0.01.
Further, in S22, the aluminum powder is uniformly sprayed into the slag liquid by rotating the lance head, so as to promote the contact between the aluminum powder and the niobium oxide in the slag layer. When the rotary gun head is used for blowing the aluminum powder, the rotary gun head keeps rotating, so that the rotary gun head plays a role in stirring in the slag liquid, the fluidity of the slag liquid is kept, and the aluminum powder is in full contact with niobium oxide in the slag liquid.
Further, the lime is roasted at high temperature to remove moisture and impurities.
The components of the niobium-iron alloy produced and prepared by the method are Nb: 60-65%, Si: 0.30-0.45%, Mn: 0.01-0.03%, C: 0.06-0.1%, S: 0.005-0.1%, P: 0.01-0.05%, W: 0.005-0.01% and the balance of iron.
Example 1
Weighing raw materials including metallurgical-grade niobium oxide, aluminum powder, ferric oxide powder, lime, fluorite powder and saltpeter, wherein the raw materials include 1000 kg, 500 kg, 400 kg, 50 kg, 60 kg and 20 kg respectively, carrying out ball milling on the lime, screening and drying for 200 ℃ for 300min, drying the aluminum powder, the fluorite powder and the saltpeter for 200 ℃ and 250min respectively, adding the materials into a reactor, igniting the materials to generate an alloy liquid and a slag liquid layer, wherein the thickness of the slag liquid layer is about 50cm, the thickness of the alloy liquid is about 40cm, pushing a reaction furnace to the position below an electrode within 2min, powering on the electrode below the electrode, blowing the aluminum powder to continuously reduce the niobium oxide in the slag liquid layer, stopping powering on after reacting for 5min, cooling and skimming the alloy liquid, cooling the alloy liquid everywhere, and sampling the alloy liquid and the slag layer.
The components of the ferrocolumbium alloy in this example were sampled and analyzed to obtain the following contents of the respective elements: nb: 63.06%, Si: 0.31%, Mn: 0.018%, C: 0.073%, S: 0.009%, P: 0.011%, W: 0.0094% and the balance of iron. The slag layer of this example was sampled and analyzed to obtain Nb as a content of each element: 1.02%, Ca: 44.32%, Al: 50.47% and the balance being iron.
Example 2
Weighing raw materials including metallurgical-grade niobium oxide, aluminum powder, ferric oxide powder, lime, fluorite powder and saltpeter, wherein the raw materials include 1000 kg, 520 kg, 420 kg, 55 kg, 63 kg and 22 kg respectively, carrying out ball milling on the lime, screening and drying for 200 ℃ for 350min, drying the aluminum powder, the fluorite powder and the saltpeter for 200 ℃ and 300min respectively, adding the materials into a reactor, igniting the materials to generate an alloy liquid and a slag liquid layer, wherein the thickness of the slag liquid layer is about 50cm, the thickness of the alloy liquid is about 40cm, pushing a reaction furnace to the position below an electrode within 2min, powering on the electrode below the electrode, blowing the aluminum powder to continuously reduce the niobium oxide in the slag liquid layer, stopping powering on after reacting for 5min, cooling and skimming the alloy liquid, cooling the alloy liquid everywhere, and sampling the alloy liquid and the slag layer.
The components of the ferrocolumbium alloy in this example were sampled and analyzed to obtain the following contents of the respective elements: nb: 62.54%, Si: 0.37%, Mn: 0.02%, C: 0.08%, S: 0.01%, P: 0.015%, W: 0.001% and the balance of iron. The slag layer of this example was sampled and analyzed to obtain Nb as a content of each element: 1.38%, Ca: 42.94%, Al: 54.15 percent and the balance of iron.
Example 3
Weighing raw materials including metallurgical-grade niobium oxide, aluminum powder, ferric oxide powder, lime, fluorite powder and saltpeter, wherein the raw materials include 1000 kg, 550 kg, 410 kg, 53 kg, 65 kg and 25 kg respectively, carrying out ball milling on the lime, screening and drying for 200 ℃ for 320min, drying the aluminum powder, the fluorite powder and the saltpeter for 200 ℃ and 320min respectively, adding the materials into a reactor, igniting the materials to generate an alloy liquid and a slag liquid layer, wherein the thickness of the slag liquid layer is about 50cm, the thickness of the alloy liquid is about 40cm, pushing a reaction furnace to the position below an electrode within 2min, powering on the electrode below the electrode, blowing the aluminum powder to continuously reduce the niobium oxide in the slag liquid layer, stopping powering on after reacting for 5min, cooling and skimming the alloy liquid, cooling the alloy liquid everywhere, and sampling the alloy liquid and the slag layer.
The components of the ferrocolumbium alloy in this example were sampled and analyzed to obtain the following contents of the respective elements: nb: 64.88%, Si: 0.42%, Mn: 0.03%, C: 0.07%, S: 0.06%, P: 0.015%, W: 0.007% and the balance of iron. The slag layer of this example was sampled and analyzed to obtain Nb as a content of each element: 1.26%, Ca: 40.65%, Al: 56.71% and the balance being iron.
It can be seen from the above examples that the niobium element in the raw material is substantially completely introduced into the ferrocolumbium alloy, and the content of niobium in the slag liquid is lower than 1.5%, which indicates that the residual niobium oxide in the slag liquid can be almost completely reduced by the method of the present invention and introduced into the alloy liquid, so that the yield of the niobium element in the raw material niobium oxide reaches 98.5%, which is much higher than the yield obtained by the aluminothermic process alone.
The above disclosure is only illustrative of the preferred embodiments of the present invention, which should not be taken as limiting the scope of the invention, but rather the invention can be embodied in other specific forms without departing from the spirit or essential characteristics thereof. It will be understood by those skilled in the art that all or a portion of the above-described embodiments may be practiced and equivalents thereof may be resorted to as falling within the scope of the invention as claimed. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A niobium-iron alloy production method is characterized by comprising the steps of producing ferrocolumbium by an aluminothermic method and refining the ferrocolumbium;
the aluminothermic method for producing the ferrocolumbium comprises the following steps:
s11: mixing the following raw materials in parts by weight:
metallurgical grade niobium oxide: aluminum powder: iron oxide powder: lime: fluorite powder: saltpeter = 1: 0.45-0.7: 0.3-0.7: 0.05-0.15: 0.06-0.2: 0.01-0.05;
s12: carrying out ball milling and particle size screening on lime in the raw materials, and controlling the particle size to be not more than 3 mm; drying the aluminum powder, the fluorite powder and the saltpeter respectively to remove water;
s13: putting the raw materials into a reactor, and igniting for reaction to obtain a ferrocolumbium alloy liquid, wherein the upper layer of the alloy liquid is a slag liquid layer;
the refining steps are as follows:
s21: placing an electrode downwards into the slag liquid layer, and heating the slag liquid layer through an electric arc to ensure that the slag liquid layer keeps fluidity;
s22: and blowing aluminum powder into the slag liquid to promote the aluminum powder to reduce the niobium element in the slag liquid out and enter the alloy liquid.
2. The niobium-iron alloy production method as claimed in claim 1, wherein: in step S13, after the internal flame of the reactor disappears and the alloy liquid becomes stable, an electrode is inserted into the alloy liquid, and the refining reaction is conducted.
3. The niobium-iron alloy production method as claimed in claim 2, wherein: the insertion depth of the electrode end is in contact with the surface of the alloy liquid, and the electrode is kept to be adjusted up and down within a small range after the current is stabilized.
4. The niobium-iron alloy production method as claimed in claim 1, wherein: when the electrode is lowered, the current is observed, when the current is instantly increased to the range of 7900 +/-100A, the electrode is kept adjusted within the range of 2-10cm above the existing height, and the current is kept stable.
5. The niobium-iron alloy production method as claimed in claim 1, wherein: in step S21, the electrode energization parameters are: voltage: 140V, current: 7900A, energization time: and 5-25 minutes, wherein the ratio of the amount of the injected aluminum powder to the amount of the niobium oxide in the slag is 1: 0.005-0.01.
6. The niobium-iron alloy production method as claimed in claim 1, wherein: in S22, the aluminum powder is uniformly sprayed into the slag liquid by rotating the gun head to promote the contact of the aluminum powder and the niobium oxide in the slag layer.
7. The niobium-iron alloy production method as claimed in claim 1, wherein: and roasting the lime at high temperature to remove moisture and impurities.
8. The niobite alloy produced by the method of any one of claims 1 to 7 having Nb: 60-65%, Si: 0.30-0.45%, Mn: 0.01-0.03%, C: 0.06-0.1%, S: 0.005-0.1%, P: 0.01-0.05%, W: 0.005-0.01% and the balance of iron.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113265572A (en) * | 2021-04-12 | 2021-08-17 | 中色（宁夏）东方集团有限公司 | Low-aluminum niobium iron and production method thereof |
| CN113943862A (en) * | 2021-11-18 | 2022-01-18 | 稀美资源(贵州)科技有限公司 | Preparation method and device of ferrocolumbium alloy |
| CN114524667A (en) * | 2021-12-30 | 2022-05-24 | 江苏新时高温材料股份有限公司 | High-stability low-cost preparation process for artificially synthesized mullite |
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| CN106591580A (en) * | 2016-11-08 | 2017-04-26 | 中色（宁夏）东方集团有限公司 | New method for preparing ferro-tungsten through low-content tungsten ore |
| CN111378883A (en) * | 2020-04-21 | 2020-07-07 | 承德天大钒业有限责任公司 | Niobium-iron intermediate alloy and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106591580A (en) * | 2016-11-08 | 2017-04-26 | 中色（宁夏）东方集团有限公司 | New method for preparing ferro-tungsten through low-content tungsten ore |
| CN111378883A (en) * | 2020-04-21 | 2020-07-07 | 承德天大钒业有限责任公司 | Niobium-iron intermediate alloy and preparation method and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113265572A (en) * | 2021-04-12 | 2021-08-17 | 中色（宁夏）东方集团有限公司 | Low-aluminum niobium iron and production method thereof |
| CN113265572B (en) * | 2021-04-12 | 2023-03-14 | 中色（宁夏）东方集团有限公司 | Low-aluminum niobium iron and production method thereof |
| CN113943862A (en) * | 2021-11-18 | 2022-01-18 | 稀美资源(贵州)科技有限公司 | Preparation method and device of ferrocolumbium alloy |
| CN114524667A (en) * | 2021-12-30 | 2022-05-24 | 江苏新时高温材料股份有限公司 | High-stability low-cost preparation process for artificially synthesized mullite |
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| CN112430756B (en) | 2023-11-28 |
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