CN104178690A - Iron-based vanadium-nitrogen microalloy additive and preparation method thereof - Google Patents

Iron-based vanadium-nitrogen microalloy additive and preparation method thereof Download PDF

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CN104178690A
CN104178690A CN201310200028.5A CN201310200028A CN104178690A CN 104178690 A CN104178690 A CN 104178690A CN 201310200028 A CN201310200028 A CN 201310200028A CN 104178690 A CN104178690 A CN 104178690A
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iron
vanadium
nitrogen
ferrovanadium
less
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CN104178690B (en
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李立英
刘立民
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SHIJIAZHUANG JINHAO NEW MATERIAL TECHNOLOGY Co Ltd
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SHIJIAZHUANG JINHAO NEW MATERIAL TECHNOLOGY Co Ltd
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Abstract

An iron-based vanadium-nitrogen microalloy additive is characterized in that by comprising the following materials by weight: 97.95 parts of 50 ferrovanadium, 2.00 parts of a combustion improver and 0.05 part of a nitriding catalyst. A preparation method comprises the steps as follows: the 50 ferrovanadium is placed in a jaw crusher (1) to be crushed into particles in particle sizes smaller than 10 millimeters; the 50 ferrovanadium particles are placed in a roll crusher (2) to be crushed; the crushed 50 ferrovanadium is placed in a ball mill (3) to be milled; the milled 50 ferrovanadium is placed in a vibrating screen (4) to be screened to obtain 50 ferrovanadium in particle sizes ranging from 120 micrometers to 180 micrometers, and 50 ferrovanadium in particle sizes smaller than or 120 micrometers; the materials are loaded into a planetary forced mixing machine (5) to be mixed uniformly; the uniformly mixed materials are loaded into graphite discs and then placed in a drying machine (6) to be dried; reaction kettles are vacuumized by a vacuum machine (9), filled with nitrogen gas from a nitrogen bottle (10), and ignited for sintering; different pressures are applied to the reaction kettles containing the materials in different particle sizes. The iron-based vanadium-nitrogen microalloy additive produced by the invention has a high vanadium-nitrogen ratio and stable ingredients and is uniform in nitrogenization.

Description

Iron-based vanadium nitrogen microalloy additive and preparation method thereof
Technical field
The invention belongs to metallic substance and preparation method, particularly a kind of iron-based vanadium nitrogen microalloy additive and preparation method thereof.
Background technology
Carrying out in the process of steel products structural adjustment, the intensity that improves straight carbon steel and micro-alloyed steel is the inevitable course, main method is wherein the research and extension that strengthens microalloyed steel, utilize micro-alloying technology, the intensity of carbon steel and micro-alloyed steel is doubled, greatly reduces the consumption of resource.In microalloyed steel, the microalloying of vanadium occupies critical role.Along with deepening continuously to VN alloy (VN) research work both at home and abroad, people are fully recognized that the beneficial effect of VN alloy, according to modern age, the research of materialogy was found, in steel after nitrogen pick-up, originally be transformed into the vanadium of precipitation state in admittedly melting the vanadium of state, given full play to the precipitation strength effect of vanadium; Nitrogen has the effect of obvious crystal grain thinning in steel; V n micro alloying is by optimizing separating out and refinement ferrite crystal grain of vanadium, give full play to the effect of grain refining strengthening and two kinds of schedule of reinforcements of precipitation strength, greatly improve the combination of strength and toughness of steel, fully demonstrated the advantage of microalloying aspect Technological Economy; Adopt v n micro alloying, do not need to add other valuable alloying elements, under hot-rolled condition, can obtain the high-strength steel that yield strength is 550-600 megapascal (MPa), therefore, VN alloy, with its significant technology economy advantage, worldwide obtains a wide range of applications.Assist the data of announcing according to middle steel, by 2010, only the total amount of niobium, vanadium, titanium micro-alloyed steel reached 7,000 ten thousand tons.Replace low intensive carbon steel with micro-alloyed steel, can reduce 25% of steel requirement.The development and improvement of micro-alloying technology, has promoted the technical progress of Iron And Steel Industry.
Iron-based vanadium nitrogen microalloy additive is a kind of important vanadium nitrogen microalloy additive, add the comprehensive mechanical properties such as wear resistance, erosion resistance, toughness, intensity, ductility, hardness and the fatigue resistance that can improve steel in steel, and make steel there is good weldability energy, and have except the effect such as inclusion, extension.Especially in high-strength low-alloy steel, the nitrogen in ferrovanadium nitride can more effectively be strengthened and crystal grain thinning than vanadium carbide, vanadium iron, saves containing vanadium raw materials, thereby reduces STEELMAKING PRODUCTION cost.Had at present several different methods to produce iron-based vanadium nitrogen microalloy additive both at home and abroad, wherein combustion synthesis method is logical people's high-pressure liquid nitrogen or nitrogen in encloses container, and the heat energy of emitting through nitrogenizing reaction makes ferrovanadium dust generate iron-based vanadium nitrogen microalloy additive.The feature of this technique is under low power consumption condition, in the short period of time, to obtain the very narrow high quality alloy of nitrogen content fluctuation range.Burning is synthetic be a kind of utilize chemical reaction self heat release continue carry out, the technology of quickly synthesized material does not need to supplement external energy in synthetic process.Also the synthetic feature of this high speed just, after building-up process combustion wave causes at the beginning, reaction is just in the unmanageable state of one.
In burning building-up process, the material self that participates in reaction can discharge enough heat energy, maintain reaction continue carry out, in building-up process, iron is not participated in reaction, vanadium burning liberated heat affects synthetic effect.In the time that in raw material, content of vanadium is too low, the heat energy that nitrogenize building-up reactions discharges be not enough to maintain nitrogenize building-up reactions continue carry out, need to add ignition dope to increase heat of reaction, but ignition dope adds too much, in synthetic process, release of heat is excessive, occurs melting metal layer, causes nitriding rate step-down, make in iron-based vanadium nitrogen microalloy additive nitrogen content unstable, also can cause the variation of product composition.Prepare in the process of iron-based vanadium nitrogen microalloy additive utilizing combustion synthesis technology, restriction quality product not only have vanadium iron and an ignition dope component proportions, also have selection and the ratio etc. of raw material granularity, size-grade distribution, nitriding temperature, nitridation time, nitrogen pressure, nitriding catalyzer.The heat dissipation environment when material combusting of different granularities is synthetic is different with nitrogen demand, and the larger material of particle size differences, in the middle of same burning situation, causes level of response to differ, and occurs the quality problems such as nitrogenize is inhomogeneous, and nitriding quality is unstable.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, provide one to utilize combustion synthesis technology, prepare vanadium nitrogen than high, stable components, the uniform iron-based vanadium of nitrogenize nitrogen microalloy additive and preparation method thereof.
The technical scheme that technical solution problem of the present invention is utilized is: a kind of iron-based vanadium nitrogen microalloy additive, is characterized in that: by weight, and 50 97.95 parts of vanadium iron, 2.00 parts of ignition dopes, 0.05 part of nitriding catalyzer.
50 described vanadium iron, are the FeV50-A of GB/T 4139-2004 vanadium iron standard or the vanadium iron of FeV50-B, and median size is 80-180 micron;
Described nitrogen, the nitrogen that is greater than 99.99% for purity;
Described ignition dope is that purity is greater than 99%, and particle diameter is the aluminium powder of 150 microns;
Described nitriding catalyzer is that purity is greater than 90%, and particle diameter is the titanium valve of 150 microns.
A preparation method for iron-based vanadium nitrogen microalloy additive, takes following steps:
A. 50 vanadium iron are put into jaw crusher broken, be broken into the little particle that is less than or equal to 10 millimeters;
B. broken vanadium iron particle being put into roll crusher further pulverizes;
C. the vanadium iron after pulverizing is put into respectively to ball mill, grind;
D. the vanadium iron after grinding is put into vibratory screening apparatus, filter out 50 vanadium iron that are less than or equal to 180 micron grain sizes, 50 vanadium iron that are greater than 180 microns are reentered in shredder and continue to grind;
E. 50 vanadium iron that are less than or equal to 180 micron grain sizes are put into vibratory screening apparatus again, filter out respectively two particle diameter grades that are less than 120-180 micron and be less than 120 microns, classification is put;
F. press different particle diameter grades, by 97.95 parts of 50 vanadium iron, 2.00 parts of ignition dope aluminium powders, 0.05 part of nitriding catalyzer titanium valve, a point footpath level installs in planet Forced Mixing machine, evenly mixes;
G. the material mixing is packed in graphite plate, put into drying machine and be dried;
H. dried material is loaded on respectively in autoclave A and autoclave B together with graphite plate, utilize vacuum machine to vacuumize autoclave, be filled with purity from nitrogengas cylinder and be greater than 99.99% high pressure nitrogen, utilize the high energy ignition unit ignition reaction in autoclave;
I. be the vanadium iron of 120-180 micron to particle diameter, reactor pressure-controlling is at 11~12mp, 120 minutes reaction times, 1700~1800 DEG C of temperature of reaction; The vanadium iron that particle diameter is less than to 120 microns, the pressure-controlling of reactor is at 8~10mp, 120 minutes reaction times, 1700~1800 DEG C of temperature of reaction;
J., after reaction finishes, reactor is decompressed to normal pressure, in the time that temperature of reaction kettle is down to below 60 DEG C, graphite plate is taken out from autoclave A and autoclave B, and the iron-based vanadium nitrogen microalloy additive after sintering is separated with graphite plate;
K. cooled iron-based vanadium nitrogen microalloy additive is carried out to fragmentation with hammer mill, particle diameter is 10~50 millimeters, and wherein particle diameter is less than 10 millimeters, is greater than 50 millimeters of footpath level sums, is not more than 6% of total amount.
The invention has the beneficial effects as follows, iron-based vanadium nitrogen microalloy additive is produced in this invention, and vanadium nitrogen is more even than high, stable components, nitrogenize.
Brief description of the drawings
Illustrate with example below in conjunction with accompanying drawing.
Figure is a kind of preparation method's of iron-based vanadium nitrogen microalloy additive FB(flow block).
In figure: 1-jaw crusher; 2-roll crusher; 3-ball mill; 4-vibratory screening apparatus; 5-planet Forced Mixing machine; 6-drying machine; 7-autoclave A; 8-autoclave B; 9-vacuum machine; 10-nitrogengas cylinder; 11-hammer mill.
Embodiment
A kind of iron-based vanadium nitrogen microalloy additive, is characterized in that: by weight, and 50 97.95 parts of vanadium iron, 2.00 parts of ignition dopes, 0.05 part of nitriding catalyzer.
50 described vanadium iron, are the FeV50-A of GB/T 4139-2004 vanadium iron standard or the vanadium iron of FeV50-B, and median size is 80-180 micron;
Described nitrogen, the nitrogen that is greater than 99.99% for purity;
Described ignition dope is that purity is greater than 99%, and particle diameter is the aluminium powder of 150 microns;
Described nitriding catalyzer is that purity is greater than 90%, and particle diameter is the titanium valve of 150 microns.
A preparation method for iron-based vanadium nitrogen microalloy additive, takes following steps:
A. 50 vanadium iron are put into jaw crusher 1 broken, be broken into the little particle that is less than or equal to 10 millimeters;
B. broken vanadium iron particle being put into roll crusher 2 further pulverizes;
C. the vanadium iron after pulverizing is put into respectively to ball mill 3, grind;
D. the vanadium iron after grinding is put into vibratory screening apparatus 4, filter out 50 vanadium iron that are less than or equal to 180 micron grain sizes, 50 vanadium iron that are greater than 180 microns are reentered in shredder 3 and continue to grind;
E. 50 vanadium iron that are less than or equal to 180 micron grain sizes are put into vibratory screening apparatus 4 again, filter out respectively two particle diameter grades that are less than 120-180 micron and be less than 120 microns, classification is put;
F. press different particle diameter grades, by 97.95 parts of 50 vanadium iron, 2.00 parts of ignition dope aluminium powders, 0.05 part of nitriding catalyzer titanium valve, a point footpath level installs in planet Forced Mixing machine 5, evenly mixes;
G. the material mixing is packed in graphite plate, put into drying machine 6 and be dried;
H. dried material is loaded on respectively in autoclave A7 and B8 together with graphite plate, utilize vacuum machine 9 to vacuumize autoclave, be filled with purity from nitrogengas cylinder 10 and be greater than 99.99% high pressure nitrogen, utilize the high energy ignition unit ignition reaction in autoclave;
I. be the vanadium iron of 120-180 micron to particle diameter, reactor pressure-controlling is at 11~12mp, 120 minutes reaction times, 1700~1800 DEG C of temperature of reaction; The vanadium iron that particle diameter is less than to 120 microns, the pressure-controlling of reactor is at 8~10mp, 120 minutes reaction times, 1700~1800 DEG C of temperature of reaction;
J., after reaction finishes, reactor is decompressed to normal pressure, in the time that temperature of reaction kettle is down to below 60 DEG C, graphite plate is taken out from autoclave A and autoclave B, and the iron-based vanadium nitrogen microalloy additive after sintering is separated with graphite plate;
K. cooled iron-based vanadium nitrogen microalloy additive is carried out to fragmentation with hammer mill 11, particle diameter is 10~50 millimeters, and wherein particle diameter is less than 10 millimeters, is greater than 50 millimeters of footpath level sums, is not more than 6% of total amount.

Claims (2)

1. an iron-based vanadium nitrogen microalloy additive, is characterized in that: by weight, and 50 97.95 parts of vanadium iron, 2.00 parts of ignition dopes, 0.05 part of nitriding catalyzer.
2. the preparation side of a kind of iron-based vanadium nitrogen microalloy additive according to claim 1, its feature is taked following steps:
A. 50 vanadium iron are put into jaw crusher (1) broken, be broken into the little particle that is less than or equal to 10 millimeters;
B. broken vanadium iron particle being put into roll crusher (2) further pulverizes;
C. the vanadium iron after pulverizing is put into respectively to ball mill (3), grind;
D. the vanadium iron after grinding is put into vibratory screening apparatus (4), filter out 50 vanadium iron that are less than or equal to 180 micron grain sizes, 50 vanadium iron that are greater than 180 microns are reentered in shredder (3) and continue to grind;
E. 50 vanadium iron that are less than or equal to 180 micron grain sizes are put into vibratory screening apparatus (4) again, filter out respectively two particle diameter grades that are less than 120-180 micron and be less than 120 microns, classification is put;
F. press different particle diameter grades, by 97.95 parts of 50 vanadium iron, 2.00 parts of ignition dope aluminium powders, 0.05 part of nitriding catalyzer titanium valve, a point footpath level installs in planet Forced Mixing machine (5), evenly mixes;
G. the material mixing is packed in graphite plate, put into drying machine (6) and be dried;
H. dried material is loaded on respectively to autoclave A(7 together with graphite plate) and autoclave B(8) in, utilize vacuum machine (9) to vacuumize autoclave, be filled with purity from nitrogengas cylinder (10) and be greater than 99.99% high pressure nitrogen, utilize the high energy ignition unit ignition reaction in autoclave;
I. be the vanadium iron of 120-180 micron to particle diameter, reactor pressure-controlling is at 11~12mp, 120 minutes reaction times, 1700~1800 DEG C of temperature of reaction; The vanadium iron that particle diameter is less than to 120 microns, the pressure-controlling of reactor is at 8~10mp, 120 minutes reaction times, 1700~1800 DEG C of temperature of reaction;
J., after reaction finishes, reactor is decompressed to normal pressure, in the time that temperature of reaction kettle is down to below 60 DEG C, graphite plate is taken out from reactor A 7 autoclave B 8, and the iron-based vanadium nitrogen microalloy additive after sintering is separated with graphite plate;
K. by cooled iron-based vanadium nitrogen for microalloy additive hammer mill (11) carry out fragmentation, particle diameter is 10~50 millimeters, wherein particle diameter is less than 10 millimeters, is greater than 50 millimeters of footpath level sums, is not more than 6% of total amount.
CN201310200028.5A 2013-05-27 2013-05-27 Iron-based vanadium-nitrogen microalloy additive and preparation method thereof Active CN104178690B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2926161B2 (en) * 1989-10-27 1999-07-28 旭化成工業株式会社 Manufacturing method of permanent magnet
CN1480548A (en) * 2003-03-13 2004-03-10 东北大学 Vanadium nitrogen microalloy additive and its preparing method
CN101693977A (en) * 2009-10-14 2010-04-14 马鞍山钢铁股份有限公司 Vanadium-nitrogen additive for smelting microalloyed steel and method for preparing same
KR20100096827A (en) * 2009-02-25 2010-09-02 현대제철 주식회사 Microalloy steel for 10t bolt, and method for producing the same
CN102828000A (en) * 2012-10-08 2012-12-19 侯巍 Metallurgical V-N microalloying and compound deoxidation cored wire

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2926161B2 (en) * 1989-10-27 1999-07-28 旭化成工業株式会社 Manufacturing method of permanent magnet
CN1480548A (en) * 2003-03-13 2004-03-10 东北大学 Vanadium nitrogen microalloy additive and its preparing method
KR20100096827A (en) * 2009-02-25 2010-09-02 현대제철 주식회사 Microalloy steel for 10t bolt, and method for producing the same
CN101693977A (en) * 2009-10-14 2010-04-14 马鞍山钢铁股份有限公司 Vanadium-nitrogen additive for smelting microalloyed steel and method for preparing same
CN102828000A (en) * 2012-10-08 2012-12-19 侯巍 Metallurgical V-N microalloying and compound deoxidation cored wire

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