CN107699780A - A kind of method for preparing ferrovanadium nitride alloy - Google Patents

A kind of method for preparing ferrovanadium nitride alloy Download PDF

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Publication number
CN107699780A
CN107699780A CN201710859074.4A CN201710859074A CN107699780A CN 107699780 A CN107699780 A CN 107699780A CN 201710859074 A CN201710859074 A CN 201710859074A CN 107699780 A CN107699780 A CN 107699780A
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ferrovanadium nitride
nitrogen
present
time
nitridation
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CN107699780B (en
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李兰杰
李九江
董自慧
吴春亮
王娜
张苏新
柳朝阳
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HBIS Co Ltd Chengde Branch
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HBIS Co Ltd Chengde Branch
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C35/00Master alloys for iron or steel
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/051Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C22C1/053Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
    • C22C1/055Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds using carbon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/16Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on nitrides

Abstract

The present invention relates to a kind of method for preparing ferrovanadium nitride alloy, methods described is:Vanadium source, carbonaceous reducing agent and iron powder are subjected to batch mixing, are then pressed into lump material;Lump material is heated and carries out carburizing reagent, is then warming up to 1,300 1500 DEG C of progress first time nitridation reactions in a nitrogen atmosphere, insulation is cooled to 1,100 1300 DEG C of progress, second of nitridation reaction after terminating, reaction obtains ferrovanadium nitride alloy after terminating.The present invention prepares high nitrogen ferrovanadium nitride using two step nitridings, and by the adjustment to temperature and nitrogen flow, the ferrovanadium nitride that nitrogen content is 14.0 15.5wt% has been prepared;The simultaneously effective purity for improving product, the content of the impurity element such as oxygen and carbon is reduced, obtained that proportion is bigger, the ferrovanadium nitride product of better quality.Present invention process process is simple, and device therefor is common, and ferrovanadium nitride preparation process energy consumption is low, has a good application prospect.

Description

A kind of method for preparing ferrovanadium nitride alloy
Technical field
The present invention relates to alloy preparation field, and in particular to a kind of method for preparing ferrovanadium nitride alloy.
Background technology
Nitrogen has excellent reinforcing effect to the Carbonitride Precipitation in micro alloyed steel.Nitrogen pick-up has following in steel Effect:(1) toughness and plasticity of steel can be obviously improved.(2) the heat resistanceheat resistant intensity and creep ability of steel can also be improved.(3) may be used To change distributing alternately for vanadium.(4) creep rupture strength of steel can be improved.At present, the method for nitriding mainly has addition to nitrogenize in steel Vanadium iron, vanadium nitride, vanadium iron, rich nitrogen ferromanganese, ferro-silicon nitride.
Ferrovanadium nitride is a kind of new VN alloy additive, and performance is better than vanadium iron and vanadium nitride, is widely used in high-strength Spend the products such as spiral, high-strength line-pipe steel, high intensity shaped steel.Ferrovanadium nitride than great, has higher suction than vanadium nitride Yield, there is the function such as higher crystal grain thinning and lifting intensity, toughness, ductility.
The existing technology for preparing ferrovanadium nitride has a lot, such as a kind of ferrovanadium nitride is disclosed in CN105483507A and is closed Barium oxide, ferriferous oxide or iron and carbonaceous reducing agent are mixed and are pressed into by gold and preparation method thereof, this method in proportion Block, it is put into high temperature furnace and carries out reaction generation ferrovanadium nitride.This method pyroreaction includes high temperature carbon thermal reduction and medium temperature nitrogenizes React two stages.The advantages of this method is that technological process is simple, but its shortcoming is that nitrogen content is relatively low in ferrovanadium nitride. Disclose a kind of ferrovanadium nitride and preparation method thereof in CN104046824A, this method by barium oxide, carbonaceous powder, iron powder, Aqueous binders and nitridation accelerator mix and are compacted into lump material, after dry materials, under the high temperature conditions, by preheating Stage, transition stage and nitridation sintered stage prepare ferrovanadium nitride.Although this method improves the content of nitrogen, but technological process phase To complexity.Disclose in CN103436770A the invention discloses a kind of preparation technology of ferrovanadium nitride, protected with nitrogen atmosphere, And pass through nitrogen clean pushed bat kiln closed bin inside and outside oxygen content be consistent, be sequentially provided with pushed bat kiln preheating zone, Area, cooling area and the region of cooling zone four are nitrogenized, 50 vanadium iron continuous conveyings that granularity is 5-20mm occur to closed bin afterwards Nitridation reaction, obtain ferrovanadium nitride.This method equally exists the problems such as complex process and relatively low nitrogen content.
In summary, it is necessary to develop that a kind of technique is simple, and the method for preparing ferrovanadium nitride alloy of nitrogen content can be improved.
The content of the invention
In view of problems of the prior art, the invention provides a kind of method for preparing ferrovanadium nitride alloy, improves Nitrogen content in ferrovanadium nitride, while the content of the impurity elements such as oxygen and carbon is reduced, improve ferrovanadium nitride proportion, gained nitrogen Change nitrogen content in vanadium iron product and reach 14.0-15.5wt%.And technological process is simple, preparation process energy consumption is low, suitable for industry Metaplasia is produced.
To use following technical scheme up to this purpose, the present invention:
The invention provides a kind of method for preparing ferrovanadium nitride alloy, the described method comprises the following steps:
(1) vanadium source, carbonaceous reducing agent and iron powder are subjected to batch mixing, are then pressed into lump material;
(2) the lump material heating obtained step (1) carries out carburizing reagent, then in a nitrogen atmosphere, is warming up to 1300-1500 DEG C of progress first time nitridation reaction, insulation are cooled to second of nitridation reaction of 1100-1300 DEG C of progress after terminating, Reaction obtains ferrovanadium nitride alloy after terminating.
The present invention prepares high nitrogen ferrovanadium nitride using two step nitridings, passes through the adjustment to temperature and nitrogen flow, system It is standby to have obtained the ferrovanadium nitride that nitrogen content is 14.0-15.5wt%, for prior art, the high nitrogen vanadium nitride of the invention prepared Iron nitrogen content improves 10% or so.
After first time nitridation reaction, nitrogen content is 11.2-13.8wt% in the ferrovanadium nitride being prepared;Second After nitridation reaction, nitrogen content has reached 14.0-15.5wt% in gained ferrovanadium nitride.
According to the present invention, based on weight/mass percentage composition, the ferrovanadium nitride alloy that step (2) obtains is composed of the following components: Vanadium 65.0-67.5%;Nitrogen 14.0-15.5%;Surplus is iron and inevitable impurity.
According to the present invention, step (1) the vanadium source be vanadium oxide, preferably V2O5、V2O3Or VO2In any one Or at least two combination, more preferably V2O3;Such as can be V2O5、V2O3Or VO2In any one, it is typical but non- What is limited is combined as V2O5And V2O3;V2O5And VO2;V2O3And VO2;V2O5、V2O3And VO2
According to the present invention, step (1) described carbonaceous reducing agent is for any one in graphite, anthracite or activated carbon or extremely Few two kinds combination, preferably graphite;Such as can be any one in graphite, anthracite or activated carbon, typical but non-limit Fixed is combined as graphite and anthracite;Graphite and activated carbon;Anthracite and activated carbon;Graphite, anthracite and activated carbon.
According to the present invention, raw material is ground before step (1) described batch mixing, the vanadium source that is obtained after grinding, carbonaceous reduction The granularity of agent and iron powder is not more than 200 μm, preferably 100-200 μm.
According to the present invention, the addition of step (1) described carbonaceous reducing agent is the 10-45wt% of vanadium source addition, such as Can be 10wt%, 15wt%, 20wt%, 25wt%, 30wt%, 35wt%, 40wt% or 45wt%, and above-mentioned numerical value it Between specific point value, as space is limited and the consideration for simplicity, the present invention no longer exclusive list.
According to the present invention, the pressure in step (1) described briquetting process is 10-15MPa, for example, can be 10MPa, 10.5MPa, 11MPa, 11.5MPa, 12MPa, 12.5MPa, 13MPa, 13.5MPa, 14MPa, 14.5MPa or 15MPa, Yi Jishang The specific point value between numerical value is stated, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the temperature of step (2) described carburizing reagent is 600-1100 DEG C, preferably 800-1000 DEG C, is entered One step is preferably 850 DEG C;Such as can be 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C, 800 DEG C, 850 DEG C, 900 DEG C, 950 DEG C, Specific point value between 1000 DEG C, 1050 DEG C or 1100 DEG C, and above-mentioned numerical value, as space is limited and for concise consideration, sheet Invention no longer exclusive list.
According to the present invention, the time of step (2) described carburizing reagent is 4-8h, for example, can be 4h, 4.5h, 5h, 5.5h, Specific point value between 6h, 6.5h, 7h, 7.5h or 8h, and above-mentioned numerical value, as space is limited and for concise consideration, this hair Bright no longer exclusive list.
According to the present invention, the temperature of step (2) the first time nitridation reaction is 1300-1500 DEG C, preferably 1400 DEG C; Such as can be 1300 DEG C, 1330 DEG C, 1350 DEG C, 1380 DEG C, 1400 DEG C, 1430 DEG C, 1450 DEG C, 1480 DEG C or 1500 DEG C, with And the specific point value between above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the time of step (2) the first time nitridation reaction is 9-13h, for example, can be 9h, 9.5h, Specific point value between 10h, 10.5h, 11h, 11.5h, 12h, 12.5h or 13h, and above-mentioned numerical value, as space is limited and for Concise consideration, the present invention no longer exclusive list.
According to the present invention, the temperature of step (2) second of nitridation reaction is 1100-1300 DEG C, preferably 1200 DEG C; Such as can be 1100 DEG C, 1130 DEG C, 1150 DEG C, 1180 DEG C, 1200 DEG C, 1230 DEG C, 1250 DEG C, 1280 DEG C or 1300 DEG C, with And the specific point value between above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
For the present invention, the temperature of first time nitridation reaction is consistently higher than second of nitridation reaction.
According to the present invention, the time of step (2) second of nitridation reaction is 10-15h, for example, can be 10h, It is specific between 10.5h, 11h, 11.5h, 12h, 12.5h, 13h, 13.5h, 14h, 14.5h or 15h, and above-mentioned numerical value Value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the flow of nitrogen is 100-350m during step (2) the first time nitridation reaction3/ h, example Such as can be 100m3/h、130m3/h、150m3/h、180m3/h、200m3/h、230m3/h、250m3/h、280m3/h、300m3/h、 330m3/ h or 350m3Specific point value between/h, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention is not Exclusive list again.
According to the present invention, the flow of nitrogen is 200-400m during step (2) second of nitridation reaction3/ h, example Such as can be 200m3/h、230m3/h、250m3/h、280m3/h、300m3/h、330m3/h、350m3/h、380m3/ h or 400m3/ Specific point value between h, and above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
The present invention is cooled down after step (2) second of nitridation reaction terminates, and the upper temp of cooling section is 800-1000 DEG C, preferably 800-900 DEG C, more preferably 850 DEG C;Such as can be 800 DEG C, 830 DEG C, 850 DEG C, 880 DEG C, 900 DEG C, 930 DEG C, 950 DEG C, 980 DEG C or the specific point value between 1000 DEG C, and above-mentioned numerical value, as space is limited and for Concise consideration, the present invention no longer exclusive list.
Temperature of lower≤200 DEG C of cooling section, it is preferably≤150 DEG C according to the present invention.
Compared with prior art, the present invention at least has the advantages that:
(1) present invention is improved by selecting nitridation reaction twice and the control to nitridation process temperature and ammonia flow Nitrogen content in ferrovanadium nitride, nitrogen content reaches 14.0-15.5wt% in gained ferrovanadium nitride product.
(2) present invention can effectively improve the pure of product by successively carrying out nitridation reaction twice after carburizing reagent Degree, the content of the impurity element such as oxygen and carbon is reduced, obtains the ferrovanadium nitride alloy product of good quality.
(3) the ferrovanadium nitride proportion that the present invention is prepared is bigger, is more beneficial for controlling the stability and accuracy of vanadium.
(4) present invention process process is simple, and device therefor is common, and ferrovanadium nitride preparation process energy consumption is low, in micro alloyed steel More it is applicable in production process.
Brief description of the drawings
Fig. 1 is the process chart that a kind of embodiment of the present invention provides.
The present invention is described in more detail below.But following examples is only the simple example of the present invention, not generation Table or limitation the scope of the present invention, protection scope of the present invention are defined by claims.
Embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by embodiment.
As shown in figure 1, the technological process that a kind of embodiment of the present invention provides can be:Vanadium source, carbonaceous are reduced It is 100-200 μm that agent and iron powder, which distinguish abrasive material to granularity, then adds batch mixer and carries out batch mixing, batch mixing terminates rear briquet Shape material;Under the atmosphere of nitrogen, obtained lump material is heated and carries out carburizing reagent, then heats to 1300-1500 DEG C First time nitridation reaction is carried out, insulation is cooled to second of nitridation reaction of 1100-1300 DEG C of progress after terminating, reaction obtains after terminating To ferrovanadium nitride alloy.
For the present invention is better described, technical scheme is readily appreciated, of the invention is typical but non-limiting Embodiment is as follows:
Embodiment 1
(1) vanadium trioxide 95.6g, graphite 27.6g, iron powder 35g are weighed, granularity is ground to respectively and is in 100-200 μm, Above-mentioned material is put into after being mixed in batch mixer and is put into briquet in cooked flake wrapping machine, pressure 12MPa;
(2) lump material that step (1) obtains is put into pushed bat kiln after drying and sieving and be fired, warm-up phase temperature Spend for 500 DEG C, time 5h, carburizing reagent phase temperature is 900 DEG C, time 6h, then passes to nitrogen, controls nitrogen flow For 250m3/ h, 1400 DEG C of progress first time nitridation reactions are warming up to, 1200 DEG C of progress, second of nitridation is cooled to after being incubated 10h Reaction, while it is 350m to control nitrogen flow3Cooling (push pedal kiln hood sets water collar) obtains vanadium nitride after/h, reaction 12h Ferroalloy, the upper temp of cooling section is 800 DEG C, temperature of lower≤150 DEG C of cooling section.
By detection, based on weight/mass percentage composition, nitrogen accounts for vanadium nitride in the ferrovanadium nitride product that the present embodiment obtains The 14.8wt% of weight of iron, v element account for the 66.2wt% of ferrovanadium nitride quality.
Embodiment 2
(1) vanadium trioxide 95.6g, graphite 25.3g, iron powder 30g are weighed, granularity is ground to respectively and is in 100-200 μm, Above-mentioned material is put into after being mixed in batch mixer and is put into briquet in cooked flake wrapping machine, pressure 13MPa;
(2) lump material that step (1) obtains is put into pushed bat kiln after drying and sieving and be fired, warm-up phase temperature Spend for 500 DEG C, time 5h, carburizing reagent phase temperature is 900 DEG C, time 6h, then passes to nitrogen, controls nitrogen flow For 250m3/ h, 1450 DEG C of progress first time nitridation reactions are warming up to, 1250 DEG C of progress, second of nitridation is cooled to after being incubated 11h Reaction, while it is 400m to control nitrogen flow3Cooling (push pedal kiln hood sets water collar) obtains vanadium nitride after/h, reaction 13h Ferroalloy, the upper temp of cooling section is 800 DEG C, temperature of lower≤150 DEG C of cooling section.
By detection, based on weight/mass percentage composition, nitrogen accounts for vanadium nitride in the ferrovanadium nitride product that the present embodiment obtains The 14.5wt% of weight of iron, v element account for the 65.8wt% of ferrovanadium nitride quality.
Embodiment 3
(1) vanadium trioxide 95.6g, graphite 32.2g, iron powder 30g are weighed, granularity is ground to respectively and is in 100-200 μm, Above-mentioned material is put into after being mixed in batch mixer and is put into briquet in cooked flake wrapping machine, pressure 15MPa;
(2) lump material that step (1) obtains is put into pushed bat kiln after drying and sieving and be fired, warm-up phase temperature Spend for 500 DEG C, time 5h, carburizing reagent phase temperature is 850 DEG C, time 6h, then passes to nitrogen, controls nitrogen flow For 150m3/ h, 1300 DEG C of progress first time nitridation reactions are warming up to, 1200 DEG C of progress, second of nitridation is cooled to after being incubated 10h Reaction, while it is 350m to control nitrogen flow3Cooling (push pedal kiln hood sets water collar) obtains vanadium nitride after/h, reaction 11h Ferroalloy, the upper temp of cooling section is 850 DEG C, temperature of lower≤150 DEG C of cooling section.
By detection, based on weight/mass percentage composition, nitrogen accounts for vanadium nitride in the ferrovanadium nitride product that the present embodiment obtains The 14.2wt% of weight of iron, v element account for the 65.7wt% of ferrovanadium nitride quality.
Embodiment 4
(1) vanadium trioxide 95.6g, graphite 31.5g, iron powder 35g are weighed, granularity is ground to respectively and is in 100-200 μm, Above-mentioned material is put into after being mixed in batch mixer and is put into briquet in cooked flake wrapping machine, pressure 12MPa;
(2) lump material that step (1) obtains is put into pushed bat kiln after drying and sieving and be fired, warm-up phase temperature Spend for 500 DEG C, time 5h, carburizing reagent phase temperature is 1000 DEG C, time 4h, then passes to nitrogen, controls nitrogen stream Measure as 200m3/ h, 1400 DEG C of progress first time nitridation reactions are warming up to, 1150 DEG C of progress, second of nitrogen is cooled to after being incubated 11h Change reaction, while it is 350m to control nitrogen flow3Cooling (push pedal kiln hood sets water collar) is nitrogenized after/h, reaction 15h Vanadium iron, the upper temp of cooling section is 850 DEG C, temperature of lower≤150 DEG C of cooling section.
By detection, based on weight/mass percentage composition, nitrogen accounts for vanadium nitride in the ferrovanadium nitride product that the present embodiment obtains The 14.4wt% of weight of iron, v element account for the 65.4wt% of ferrovanadium nitride quality.
Embodiment 5
(1) vanadium trioxide 95.6g, graphite 27.6g, iron powder 35g are weighed, granularity is ground to respectively and is in 100-200 μm, Above-mentioned material is put into after being mixed in batch mixer and is put into briquet in cooked flake wrapping machine, pressure 12MPa;
(2) lump material that step (1) obtains is put into pushed bat kiln after drying and sieving and be fired, warm-up phase temperature Spend for 500 DEG C, time 5h, carburizing reagent phase temperature is 850 DEG C, time 7h, then passes to nitrogen, controls nitrogen flow For 100m3/ h, 1450 DEG C of progress first time nitridation reactions are warming up to, 1200 DEG C of progress, second of nitridation is cooled to after being incubated 13h Reaction, while it is 400m to control nitrogen flow3Cooling (push pedal kiln hood sets water collar) obtains vanadium nitride after/h, reaction 13h Ferroalloy, the upper temp of cooling section is 850 DEG C, temperature of lower≤150 DEG C of cooling section.
By detection, based on weight/mass percentage composition, nitrogen accounts for vanadium nitride in the ferrovanadium nitride product that the present embodiment obtains The 14.6wt% of weight of iron, v element account for the 66.1wt% of ferrovanadium nitride quality.
Embodiment 6
(1) vanadium trioxide 95.6g, graphite 25.3g, iron powder 35g are weighed, granularity is ground to respectively and is in 100-200 μm, Above-mentioned material is put into after being mixed in batch mixer and is put into briquet in cooked flake wrapping machine, pressure 12MPa;
(2) lump material that step (1) obtains is put into pushed bat kiln after drying and sieving and be fired, warm-up phase temperature Spend for 500 DEG C, time 5h, carburizing reagent phase temperature is 650 DEG C, time 8h, then passes to nitrogen, controls nitrogen flow For 150m3/ h, 1500 DEG C of progress first time nitridation reactions are warming up to, 1300 DEG C of progress, second of nitridation is cooled to after being incubated 12h Reaction, while it is 300m to control nitrogen flow3Cooling (push pedal kiln hood sets water collar) obtains vanadium nitride after/h, reaction 12h Ferroalloy, the upper temp of cooling section is 850 DEG C, temperature of lower≤150 DEG C of cooling section.
By detection, based on weight/mass percentage composition, nitrogen accounts for vanadium nitride in the ferrovanadium nitride product that the present embodiment obtains The 14.3wt% of weight of iron, v element account for the 65.9wt% of ferrovanadium nitride quality.
Comparative example 1
Compared with Example 1, except directly cooling obtains ferrovanadium nitride alloy after first time nitridation reaction in step (2) Outside, other conditions are identical with embodiment 1.(only carrying out first time nitridation reaction)
By detection, based on weight/mass percentage composition, nitrogen accounts for vanadium nitride in the ferrovanadium nitride product that this comparative example obtains The 13.6wt% of weight of iron, v element account for the 66.5wt% of ferrovanadium nitride quality.
Comparative example 2
Compared with Example 1, except without first time nitridation reaction, i.e., directly being carried out after carburizing reagent in step (2) 1200 DEG C are warming up to, it is 350m to control nitrogen flow3/ h, second of nitridation reaction is carried out, is cooled down after reaction 12h and obtains vanadium nitride Outside ferroalloy, other conditions are identical with embodiment 1.(only carrying out second of nitridation reaction)
By detection, based on weight/mass percentage composition, nitrogen accounts for vanadium nitride in the ferrovanadium nitride product that this comparative example obtains The 12.9wt% of weight of iron, v element account for the 66.9wt% of ferrovanadium nitride quality.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should equally be considered as content disclosed in this invention.

Claims (10)

  1. A kind of 1. method for preparing ferrovanadium nitride alloy, it is characterised in that the described method comprises the following steps:
    (1) vanadium source, carbonaceous reducing agent and iron powder are subjected to batch mixing, are then pressed into lump material;
    (2) the lump material heating obtained step (1) carries out carburizing reagent, then in a nitrogen atmosphere, is warming up to 1300- 1500 DEG C of progress first time nitridation reactions, insulation are cooled to second of nitridation reaction of 1100-1300 DEG C of progress, reaction knot after terminating Ferrovanadium nitride alloy is obtained after beam.
  2. 2. the method as described in claim 1, it is characterised in that based on weight/mass percentage composition, ferrovanadium nitride that step (2) obtains Alloy is composed of the following components:Vanadium 65.0-67.5%;Nitrogen 14.0-15.5%;Surplus is iron and inevitable impurity.
  3. 3. the method as described in claim 1, it is characterised in that step (1) the vanadium source be vanadium oxide, preferably V2O5、 V2O3Or VO2In any one or at least two combination, more preferably V2O3
    Preferably, step (1) described carbonaceous reducing agent is any one in graphite, anthracite or activated carbon or at least two Combination, preferably graphite.
  4. 4. the method as described in claim 1, it is characterised in that be ground before step (1) described batch mixing to raw material, after grinding The granularity of obtained vanadium source, carbonaceous reducing agent and iron powder is not more than 200 μm, preferably 100-200 μm.
  5. 5. the method as described in claim 1, it is characterised in that the addition of step (1) described carbonaceous reducing agent is that vanadium source adds Enter the 10-45wt% of amount.
  6. 6. the method as described in claim 1, it is characterised in that the pressure in step (1) described briquetting process is 10-15MPa.
  7. 7. the method as described in claim 1, it is characterised in that the temperature of step (2) described carburizing reagent is 600-1100 DEG C, Preferably 800-1000 DEG C, more preferably 850 DEG C;
    Preferably, the time of step (2) described carburizing reagent is 4-8h.
  8. 8. the method as described in claim 1, it is characterised in that the temperature of step (2) the first time nitridation reaction is 1400 ℃;
    Preferably, the time of step (2) the first time nitridation reaction is 9-13h;
    Preferably, the temperature of step (2) second of nitridation reaction is 1200 DEG C;
    Preferably, the time of step (2) second of nitridation reaction is 10-15h.
  9. 9. the method as described in claim 1, it is characterised in that nitrogen during step (2) the first time nitridation reaction Flow is 100-350m3/h;
    Preferably, the flow of nitrogen is 200-400m during step (2) second of nitridation reaction3/h。
  10. 10. the method as described in claim 1, it is characterised in that step (2) second of nitridation reaction carries out cold after terminating But, the upper temp of cooling section is 800-1000 DEG C, preferably 800-900 DEG C, more preferably 850 DEG C;
    Preferably, temperature of lower≤200 DEG C of cooling section, it is preferably≤150 DEG C.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109097616A (en) * 2018-09-07 2018-12-28 河钢股份有限公司承德分公司 A kind of device and method of continuous production ferrovanadium nitride alloy
CN109855931A (en) * 2018-12-20 2019-06-07 河钢股份有限公司 A kind of preparation method of austenitic alloy EBSD sample
CN110923557A (en) * 2019-10-30 2020-03-27 中色(宁夏)东方集团有限公司 Preparation method of high-density nitrided ferrovanadium
CN113604696A (en) * 2021-08-09 2021-11-05 宁夏中宏氮化制品有限公司 Method for preparing silicon nitride ferrovanadium by vacuum resistance method
CN113652570A (en) * 2021-08-20 2021-11-16 湖南众鑫新材料科技股份有限公司 Process for increasing nitrogen content of vanadium nitride iron
CN113930661A (en) * 2021-08-10 2022-01-14 河钢承德钒钛新材料有限公司 Preparation method of nitrided ferrovanadium alloy additive
CN114873569A (en) * 2022-06-15 2022-08-09 昆明理工大学 Method for preparing high-quality vanadium nitride by vanadium oxide reduction nitridation under reducing atmosphere
CN115522092A (en) * 2022-10-25 2022-12-27 河南昱千鑫金属科技有限公司 Production method of high-nitrogen low-carbon vanadium-nitrogen alloy

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CN106834775A (en) * 2016-11-24 2017-06-13 北京科技大学 A kind of carbon thermal reduction and the method for Nitration synthesis ferrovanadium nitride
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109097616A (en) * 2018-09-07 2018-12-28 河钢股份有限公司承德分公司 A kind of device and method of continuous production ferrovanadium nitride alloy
CN109097616B (en) * 2018-09-07 2020-12-01 河钢股份有限公司承德分公司 Device and method for continuously producing nitrided ferrovanadium alloy
CN109855931A (en) * 2018-12-20 2019-06-07 河钢股份有限公司 A kind of preparation method of austenitic alloy EBSD sample
CN110923557A (en) * 2019-10-30 2020-03-27 中色(宁夏)东方集团有限公司 Preparation method of high-density nitrided ferrovanadium
CN113604696A (en) * 2021-08-09 2021-11-05 宁夏中宏氮化制品有限公司 Method for preparing silicon nitride ferrovanadium by vacuum resistance method
CN113930661A (en) * 2021-08-10 2022-01-14 河钢承德钒钛新材料有限公司 Preparation method of nitrided ferrovanadium alloy additive
CN113652570A (en) * 2021-08-20 2021-11-16 湖南众鑫新材料科技股份有限公司 Process for increasing nitrogen content of vanadium nitride iron
CN114873569A (en) * 2022-06-15 2022-08-09 昆明理工大学 Method for preparing high-quality vanadium nitride by vanadium oxide reduction nitridation under reducing atmosphere
CN115522092A (en) * 2022-10-25 2022-12-27 河南昱千鑫金属科技有限公司 Production method of high-nitrogen low-carbon vanadium-nitrogen alloy
CN115522092B (en) * 2022-10-25 2023-10-13 河南昱千鑫金属科技有限公司 Production method of high-nitrogen low-carbon vanadium-nitrogen alloy

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