CN107419157A - A kind of method that pure iron smelting Nd Fe B alloys is substituted with reduced iron powder - Google Patents

A kind of method that pure iron smelting Nd Fe B alloys is substituted with reduced iron powder Download PDF

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CN107419157A
CN107419157A CN201710451419.2A CN201710451419A CN107419157A CN 107419157 A CN107419157 A CN 107419157A CN 201710451419 A CN201710451419 A CN 201710451419A CN 107419157 A CN107419157 A CN 107419157A
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iron powder
reduced iron
alloys
briquetting
reduced
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CN107419157B (en
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郭长庆
曹杰瑞
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Jiangsu University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/04Making ferrous alloys by melting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Power Engineering (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The present invention relates to Nd Fe B alloys preparing technical field, refers in particular to a kind of method that pure iron smelting Nd Fe B alloys is substituted with reduced iron powder.The raw material that reduced iron powder is used as preparing Nd Fe B alloys needs to be pressed into stub briquetting before, and this stub briquetting is identical when its smelting process is with using pure iron as raw material during melting Nd Fe B alloys in vaccum sensitive stove.Because the chemical composition of high-purity reduced iron powder is close with pure iron, also, degree of purity is higher, and price is also than less expensive.So substitute pure iron using high-purity reduced iron powder briquetting is not only able to ensure the quality of neodymium iron boron as the raw material of production Nd Fe B alloys, moreover, it is also possible to be effectively reduced its production cost.Production practices show:The magnetic energy product that the sintered Nd-Fe-B alloy of pure iron production is substituted using reduced iron powder briquetting reaches 55 65MGoe, with using same process suitable as the Nd Fe B alloys that raw material produces using pure iron.

Description

A kind of method that pure iron smelting Nd Fe B alloys is substituted with reduced iron powder
Technical field
The present invention relates to Nd Fe B alloys preparing technical field, refers in particular to one kind reduced iron powder and substitutes pure iron smelting neodymium iron boron The method of alloy, belong to metallurgical engineering field.
Background technology
Nd Fe B alloys is as third generation rare earth permanent-magnetic material, with magnetic energy product is high, coercivity is strong, small volume, light weight It is widely used in telecommunications, Aero-Space, transportation and energy, health care, computer with the distinguishing feature such as cost performance height And the field such as household electrical appliance.
It is to produce the first step of neodymium-iron-boron magnetic material that vacuum melting is carried out in vacuum induction furnace, and the purpose of melting is Prepare Nd Fe B alloys ingot.In Nd Fe B alloys, Fe elements generally account for the 55-60wt% of alloying component, and pure iron is currently The most important supplier of Fe elements.Production practices show:The purity of pure iron is higher, and the impurity content such as C, Si, Mn, S, P is got over Low, then the magnetic property for the Nd Fe B alloys produced is better.So select high cleanliness pure iron prepare Nd Fe B alloys for The performance for improving Nd Fe B alloys is significant.
The production technology of modern pure iron and common carbon steel production technology are essentially identical, i.e.,:First in converter fusing and The raw material that is made up of molten iron and steel scrap blow to obtain primary pure iron liquation.Then, primary liquation is transferred to LF stoves, VOD stoves Or AOD argon oxygen decarburizing furnaces carry out deep desulfurization, deep decarburization, deoxidation and degassing refining treatment.When the composition and temperature of pure iron liquation reach To after requiring, it is cast as to square billet or round billet steel ingot on conticaster.Steel ingot is cooled to after room temperature or still in Warm status When, it is transported to the heating of heating furnace high temperature and reaches rolling temperature.Afterwards, being transported to rolling in rolling mill turns intoElongated bar.Elongated bar turns into by shear treatmentStub, become smelting The raw material of Nd Fe B alloys.Because pure iron phosphorus content is extremely low, C≤0.02wt%, so, the temperature of smelting ferroferrite liquation is far high In the temperature of smelting low carbon steel molten steel, its result necessarily cause smelting ferroferrite converter and refining furnace furnace lining melting loss it is serious, stove The service life degradation of son.Also, modern pure iron technological process of production length so that its production cost is high.In addition, smelt pure One of raw material of iron-blast-melted, reduction temperature is high during its acquisition, can not only reduce the iron oxide in Iron concentrate, Moreover, some other impurity elements contained in ore can also be reduced and made it into molten iron.The raw material of smelting ferroferrite it Two-steel scrap, itself wide material sources, often it is entrained with a certain amount of alloy wasting steel.Closed in these alloy wasting steels containing substantial amounts of Gold element, it can enter in subsequent smelting process in pure iron liquation and turn into impurity element.Therefore, modern pure iron production technology It is difficult to ensure that the iron-bearing material for obtaining high cleanliness.
Hyperpure iron extract is a kind of using iron oxide as the extremely low pure fine iron breeze of other impurities content of advocating peace.Ultra pure iron essence Powder is by carbon is once reduced directly and passed through in hydrogen reducing furnace the deep decarburization of wet hydrogen progress in tunnel cave and desulfurization is secondary Acquisition C, Si, Mn, S, P and the reduced iron powder that other impurities constituent content is extremely low, degree of purity is high after processing.Because The temperature that carbon is once reduced directly in tunnel cave is less than 1300 DEG C, and deep decarburization and desulfurization are carried out with wet hydrogen in hydrogen reducing furnace The temperature of after-treatment is less than 1000 DEG C, and two technical process are all to carry out in the solid state, and its temperature is far below blast furnace ironmaking temperature Spend and bessemerize the temperature of primary pure iron liquation.Therefore, the more primary pure iron liquation of amount that impurity element enters in reduced iron powder Much less, its degree of purity is much better than pure iron naturally.
However, high-purity small (1.5g-2.0g/cm of reduced iron powder proportion3), light weight, volume it is big, smelting should not be directly used as The iron-bearing material for refining Nd Fe B alloys uses.By adding a small amount of binding agent in high-purity reduced iron powder and being pressed with mould Proportion 6.5g-7.2g/cm is made3Hyperbaric stub briquetting product can transform into former for the high-quality iron content of similar pure iron block Material.Because high-purity reduced iron powder stub briquetting quality of item is excellent, production cost is low, therefore, it is a kind of more satisfactory replacement is pure Novel iron-containing raw material of the iron as production Nd Fe B alloys.
The content of the invention
1st, high-purity reduced iron powder briquetting is used to substitute the process of pure iron smelting Nd Fe B alloys for raw material, its feature exists In:
(1) raw material for preparing reduced iron powder briquetting is hyperpure iron extract, its chemical composition:TFe >=70wt%, it is low-phosphorous (P≤ 0.003wt%) and low-sulfur (S≤0.03wt%).
(2) hyperpure iron extract in tunnel cave high temperature carbon by being once reduced directly and passing through wet hydrogen in hydrogen reducing furnace The deep decarburization of gas (vapor+hydrogen gas mixture), desulfurization after-treatment are changed into high-purity reduced iron powder.Reduced during after-treatment Thickness of feed layer 50-60mm, 930 DEG C -970 DEG C, soaking time 100-120min of high temperature section temperature, reducing gas flow are controlled in stove 100-120m3/ h, wherein, water vapour content 10-12% in wet hydrogen.The chemistry of the reduced iron powder obtained after after-treatment Composition is:TFe >=99.5wt%, C≤0.0015wt%, Si≤0.15wt%, Mn≤0.15wt%, P≤0.003wt%, S≤ 0.002wt%.
(3) reduced iron powder agglomates is poured into sand mixer for casting and rolls, grinds.Added in process of lapping and account for reduced iron powder weight Measure 0.5-1wt% sodium silicate binder and 2-3wt% water to mix with reduced iron powder, and mix wet feed;
(4) reduced iron powder wet feed is poured intoStub mould in, pressed under 600MPa pressure Proportion 6.8g-7.2g/cm is made3Stub briquetting.Afterwards, stub briquetting is dried at degasification at 200 DEG C -250 DEG C 2-3 hours are managed, thoroughly to remove moisture contained therein.
(5) the melting Nd Fe B alloys in vacuum induction furnace.Before energization starts, by reduced iron powder briquetting, neodymium metal and Ferro-boron is added in crucible together.Then, vacuumize, the melting batch under high vacuum state.Constantly added in fusion process Remaining reduced iron powder briquetting and other raw metals, it is identical when its smelting process using pure iron with being smelted.
(6) production practices prove:The sintered Nd-Fe-B alloy for using reduced iron powder briquetting to produce for pure iron for raw material Magnetic energy product reaches 55-65MGoe, is that pure iron compares with using same process suitable as the Nd Fe B alloys that raw material produces using pure iron Preferable substitute.
Brief description of the drawings
Fig. 1 is flow chart of the present invention.
Embodiment
The chemical composition of the ultrapure iron concentrate powder of selection is:TFe 71.5wt%, P 0.003wt%, S 0.01wt%, SiO20.015wt%.According to prepare the common process of reduced iron powder by ultrapure iron concentrate powder pyrocarbon one first in tunnel cave Secondary direct-reduction.Then, it is secondary by the deep decarburization of wet hydrogen (vapor+hydrogen gas mixture), desulfurization in hydrogen reducing furnace Processing is changed into high-purity reduced iron powder.During after-treatment in reduction furnace control thickness of feed layer 55mm, 960 DEG C of high temperature section temperature, Soaking time 120min, reducing gas flow 120m3/ h, wherein, water vapour content 12% in wet hydrogen.High-purity reduced iron powder Chemical composition be:TFe 99.5wt%, C0.0012wt%, Si 0.013wt%, Mn0.035%wt, P 0.002wt%, S 0.0015wt%.
High-purity reduced iron powder agglomates is poured into sand mixer for casting and rolls and grinds.Add 1wt%'s in process of lapping Reduced iron powder is mixed wet feed by water glass solution and 3wt% water.Wet feed is poured into mould and is pressed intoProportion About 6.8g/cm3Stub briquetting.Afterwards, stub briquetting is dried 3 hours at 250 DEG C, thoroughly to remove water contained therein Point.
Nd Fe B alloys is smelted in 0.5 ton of vacuum induction furnace.Ferro-boron and rare earth are put into crucible.Then, reduced iron is used Powder stub briquetting fills up crucible.Vacuumize, be powered melting batch when vacuum reaches 0.05Pa.When furnace charge all melts hinterland It is continuous to add remaining metal charge and continue to heat up.Alloy is poured into a mould after temperature reaches requirement.Then, according to preparing neodymium-iron-boron Property material the next step processing alloy cast ingot.Production practices prove:Use reduced iron powder briquetting to replace to give birth to for pure iron for raw material The magnetic energy product of the sintered Nd-Fe-B alloy of the Nd Fe B alloys of production reaches 60Mgoe, with using same process to be given birth to by raw material of pure iron The Nd Fe B alloys of production is suitable, is the more satisfactory substitute of pure iron.

Claims (4)

  1. A kind of 1. method that pure iron smelting Nd Fe B alloys is substituted with reduced iron powder, it is characterised in that:Hyperpure iron extract is passed through Once it is reduced directly in tunnel cave high temperature carbon and changes in hydrogen reducing furnace by the decarburization of wet hydrogen depth, desulfurization after-treatment For high-purity reduced iron powder;Stub briquetting is pressed into after reduced iron powder addition sodium silicate binder and water are mixed into wet feed, removes stub Contained moisture in briquetting;The melting Nd Fe B alloys in vacuum induction furnace, before energization starts, by reduced iron powder briquetting, gold Category neodymium and ferro-boron are added in crucible together, then, are vacuumized, the melting batch under high vacuum state, in fusion process constantly Remaining reduced iron powder briquetting and other raw metals are added in ground, identical when its smelting process using pure iron with being smelted.
  2. A kind of 2. method that pure iron smelting Nd Fe B alloys is substituted with reduced iron powder as claimed in claim 1, it is characterised in that: The chemical composition of the hyperpure iron extract is:TFe >=70wt%, low-phosphorous P≤0.003wt% and low-sulfur S≤0.03wt%.
  3. A kind of 3. method that pure iron smelting Nd Fe B alloys is substituted with reduced iron powder as claimed in claim 1, it is characterised in that It is described that hyperpure iron extract is deep by being once reduced directly in tunnel cave high temperature carbon and passing through wet hydrogen in hydrogen reducing furnace Decarburization, desulfurization after-treatment are changed into high-purity reduced iron powder and are:Thickness of feed layer 50- is controlled during after-treatment in reduction furnace 60mm, 930 DEG C -970 DEG C, soaking time 100-120min of high temperature section temperature, reducing gas flow 100-120m3/ h, wherein, it is wet Water vapour content 10-12% in hydrogen;The chemical composition of the reduced iron powder obtained after after-treatment is:TFe≥ 99.5wt%, C≤0.0015wt%, Si≤0.15wt%, Mn≤0.15wt%, P≤0.003wt%, S≤0.002wt%.
  4. A kind of 4. method that pure iron smelting Nd Fe B alloys is substituted with reduced iron powder as claimed in claim 1, it is characterised in that Stub briquetting is pressed into after reduced iron powder addition sodium silicate binder and water are mixed into wet feed, removes moisture contained in stub briquetting For:Reduced iron powder agglomates is poured into sand mixer for casting and rolls, grind, is added in process of lapping and accounts for reduced iron powder weight 0.5- 1wt% sodium silicate binder and 2-3wt% water mix with reduced iron powder, and mix wet feed;Reduced iron powder wet feed is poured intoStub mould in, proportion 6.8g-7.2g/cm is compressed under 600MPa pressure3Stub pressure Block, afterwards, stub briquetting is dried to degassing processing 2-3 hours at 200 DEG C -250 DEG C, it is contained therein thoroughly to remove Moisture.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113724958A (en) * 2021-08-31 2021-11-30 安徽工业大学 Preparation method for producing iron-based soft magnetic iron core based on reduced iron powder alloying

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113724958A (en) * 2021-08-31 2021-11-30 安徽工业大学 Preparation method for producing iron-based soft magnetic iron core based on reduced iron powder alloying
CN113724958B (en) * 2021-08-31 2024-04-16 安徽工业大学 Preparation method for producing iron-based soft magnetic iron core based on reduced iron powder alloying

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