CN104178690B - Iron-based vanadium-nitrogen microalloy additive and preparation method thereof - Google Patents
Iron-based vanadium-nitrogen microalloy additive and preparation method thereof Download PDFInfo
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- CN104178690B CN104178690B CN201310200028.5A CN201310200028A CN104178690B CN 104178690 B CN104178690 B CN 104178690B CN 201310200028 A CN201310200028 A CN 201310200028A CN 104178690 B CN104178690 B CN 104178690B
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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
Technical field
The invention belongs to metal material and preparation method, particularly to a kind of iron-based vanadium nitrogen microalloy additions and its preparation
Method.
Background technology
During carrying out steel products structural adjustment, improving straight carbon steel and the intensity of micro alloyed steel is only way,
Main method therein is to increase the research and extension of micro alloyed steel, using micro-alloying technology, makes carbon steel and microalloy
The intensity of steel is doubled, and greatly reduces the consumption of resource.In micro alloyed steel, the microalloying of vanadium occupies critical role.With
And both at home and abroad VN alloy (VN) research work is deepened continuously, people are fully recognized that the beneficial effect of VN alloy, according to
The research of modern age materialogy finds, after nitrogen pick-up in steel, the vanadium being originally in admittedly molten state is transformed into the vanadium of precipitation state, fully sends out
Wave the precipitation enhancement of vanadium；Nitrogen has the effect of obvious crystal grain thinning in steel；V n micro alloying passes through to optimize vanadium
Precipitation and fining ferrite grains, given full play to grain refining strengthening and the effect of two kinds of schedule of reinforcements of precipitation strength, greatly
Improve greatly the combination of strength and toughness of steel, fully demonstrate advantage in terms of Technological Economy for the microalloying；Using vanadium nitrogen microalloy
Change it is not necessary to add other valuable alloying elements, can obtain yield strength under hot-rolled condition is 550-600 megapascal (MPa)
High strength steel, therefore, VN alloy, with its significant technology economy advantage, worldwide obtains a wide range of applications.
The data announced according to middle steel association, by 2010, only niobium, vanadium, the total amount of titanium micro-alloyed steel reached 70,000,000 tons.Use microalloy
Steel replaces low intensive carbon steel, can reduce the 25% of steel requirement.The development of micro-alloying technology and perfect, has promoted steel
The technological progress of ironworker's industry.
Iron-based vanadium nitrogen microalloy additions are a kind of important vanadium nitrogen microalloy additions, add in steel and can improve the resistance to of steel
The comprehensive mechanical properties such as mill property, corrosion resistance, toughness, intensity, ductility, hardness and fatigue resistance, and it is good so that steel is had
Solderable performance, and have except the effect such as field trash, extension.Especially in Aldecor, in ferrovanadium nitride
Nitrogen can more effectively be strengthened and crystal grain thinning than vanadium carbide, vanadium iron, save and contain vanadium raw materials, thus reducing STEELMAKING PRODUCTION cost.
Multiple methods have been had to produce iron-based vanadium nitrogen microalloy additions both at home and abroad at present, wherein combustion synthesis method is in closed container
Logical people's high-pressure liquid nitrogen or nitrogen, the heat energy released through nitridation reaction makes ferrovanadium dust generate the interpolation of iron-based vanadium nitrogen microalloy
Agent.The feature of this technique is to can get the very narrow high-quality alloy of nitrogen content fluctuation range in the short time under the conditions of low power consumption.
Conbustion synthesis are a kind of persistently carrying out using chemical reaction self-heat generation, the technology of quickly synthesized material, in the process of synthesis
In do not require supplementation with external energy.Also the feature of exactly this high speed synthesis, after building-up process combustion wave causes at the beginning, instead
A kind of unmanageable state should be at.
During conbustion synthesis, the material itself participating in reaction can discharge enough heat energy, maintains persistently entering of reaction
OK, in building-up process, reaction do not participated in by iron, and vanadium burning liberated heat affects synthetic effect.When in raw material, content of vanadium is too low
When, the discharged heat energy of Nitration synthesis reaction is not enough to maintain persistently carrying out of Nitration synthesis reaction, needs to add combustion adjuvant to increase
Plus heat of reaction, but combustion adjuvant adds excessively, and during synthesis, release heat is excessive, melting metal layer, causes to nitrogenize
Rate step-down, makes that in iron-based vanadium nitrogen microalloy additions, nitrogen content is unstable, also results in the change of product composition.Using burning
During synthetic technology prepares iron-based vanadium nitrogen microalloy additions, not only vanadium iron and the combustion adjuvant composition of limit product quality
Ratio, also raw material granularity, size distribution, nitriding temperature, nitridation time, nitrogen pressure, the selection of nitriding catalyst and ratio
Deng.Heat dissipation environment during the material combusting synthesis of different granularities is different with nitrogen demand, and the larger material of particle size differences is same
In the middle of one burning situation, cause the extent of reaction to differ, occur that nitridation is uneven, the quality problems such as nitriding quality is unstable.
Content of the invention
It is an object of the invention to overcoming above-mentioned deficiency, providing one kind to utilize combustion synthesis technology, preparing vanadium nitrogen than high, one-tenth
Divide and stablize, nitrogenize uniform iron-based vanadium nitrogen microalloy additions and preparation method thereof.
The present invention solve technical problem using technical scheme be：A kind of iron-based vanadium nitrogen microalloy additions, its feature
It is：By weight, 97.95 parts of 50 vanadium iron, 2.00 parts of combustion adjuvant, 0.05 part of nitriding catalyst.
50 described vanadium iron, are the vanadium iron of FeV50-A or FeV50-B of GB/T 4139-2004 vanadium iron standard, average grain
Footpath is 80-180 micron；
Described nitrogen, is the nitrogen that purity is more than 99.99%；
Described combustion adjuvant is more than 99% for purity, and particle diameter is 150 microns of aluminium powder；
Described nitriding catalyst is more than 90% for purity, and particle diameter is 150 microns of titanium valve.
A kind of preparation method of iron-based vanadium nitrogen microalloy additions, takes following steps：
A. 50 vanadium iron are put into broken in jaw crusher, be broken into the particle less than or equal to 10 millimeters；
B. broken vanadium iron particle is put in double-roll crusher and pulverize further；
C. the vanadium iron after pulverizing is respectively put in ball mill, is ground；
D. the vanadium iron after grinding is put in vibratory sieve, filter out 50 vanadium iron less than or equal to 180 micron grain sizes, will be greater than
180 microns of 50 vanadium iron are reentered in ball mill and continue to grind；
E. 50 vanadium iron less than or equal to 180 micron grain sizes are placed again in vibratory sieve, filter out 120-180 micron respectively
With two particle diameter grades less than 120 microns, classification storing；
F. different particle diameter grades are pressed, by 97.95 parts of 50 vanadium iron, 2.00 parts of combustion adjuvant aluminium powder, nitriding catalyst titanium valve
0.05 part, a point footpath level is attached in planet Forced Mixing machine, uniformly mixes；
G. the material mixing is loaded in graphite plate, put in drying machine and be dried；
H. dried material is loaded in autoclave A and autoclave B respectively together with graphite plate, using vacuum
Machine vacuumizes to autoclave, after nitrogen cylinder is filled with the high pressure nitrogen that purity is more than 99.99%, using in autoclave
High energy ignition unit ignition reaction；
I. to particle diameter for 120-180 micron vanadium iron, reactor pressure controls in 11～12MPa, 120 points of reaction time
Clock, 1700～1800 DEG C of reaction temperature；Particle diameter is less than with 120 microns of vanadium iron, the Stress control of reactor in 8～10MPa, instead
120 minutes between seasonable, 1700～1800 DEG C of reaction temperature；
J., after reaction terminates, reactor is decompressed to normal pressure, when temperature of reaction kettle is down to below 60 DEG C, graphite plate from height
Take out in pressure reactor A and autoclave B, the iron-based vanadium nitrogen microalloy additions after sintering are separated with graphite plate；
K. the iron-based vanadium nitrogen microalloy additions after cooling are crushed with hammer mill, particle diameter is 10～50 millis
Rice, wherein particle diameter are less than 10 millimeters, more than 50 millimeters of footpath level sums, no more than the 6% of total amount.
The invention has the beneficial effects as follows, iron-based vanadium nitrogen microalloy additions are produced in this invention, and vanadium nitrogen is more steady than high, composition
Fixed, nitridation is uniform.
Brief description
Illustrated with example below in conjunction with accompanying drawing.
Figure is a kind of FB(flow block) of the preparation method of iron-based vanadium nitrogen microalloy additions.
In figure：1- jaw crusher；2- double-roll crusher；3- ball mill；4- vibratory sieve；5- planet Forced Mixing machine；6-
Drying machine；7- autoclave A；8- autoclave B；9- vacuum machine；10- nitrogen cylinder；11- hammer mill.
Specific embodiment
A kind of iron-based vanadium nitrogen microalloy additions it is characterised in that：By weight, 97.95 parts of 50 vanadium iron, combustion adjuvant 2.00
Part, 0.05 part of nitriding catalyst.
50 described vanadium iron, are the vanadium iron of FeV50-A or FeV50-B of GB/T 4139-2004 vanadium iron standard, average grain
Footpath is 80-180 micron；
Described nitrogen, is the nitrogen that purity is more than 99.99%；
Described combustion adjuvant is more than 99% for purity, and particle diameter is 150 microns of aluminium powder；
Described nitriding catalyst is more than 90% for purity, and particle diameter is 150 microns of titanium valve.
A kind of preparation method of iron-based vanadium nitrogen microalloy additions, takes following steps：
A. 50 vanadium iron are put into broken in jaw crusher 1, be broken into the particle less than or equal to 10 millimeters；
B. broken vanadium iron particle is put in double-roll crusher 2 and pulverize further；
C. the vanadium iron after pulverizing is respectively put in ball mill 3, is ground；
D. the vanadium iron after grinding is put in vibratory sieve 4, filter out 50 vanadium iron less than or equal to 180 micron grain sizes, will be big
It is reentered in ball mill 3 in 180 microns of 50 vanadium iron and continue to grind；
E. 50 vanadium iron less than or equal to 180 micron grain sizes are placed again in vibratory sieve 4, filter out 120-180 respectively micro-
Rice and two particle diameter grades less than 120 microns, classification is put；
F. different particle diameter grades are pressed, by 97.95 parts of 50 vanadium iron, 2.00 parts of combustion adjuvant aluminium powder, nitriding catalyst titanium valve
0.05 part, a point footpath level is attached in planet Forced Mixing machine 5, uniformly mixes；
G. the material mixing is loaded in graphite plate, put in drying machine 6 and be dried；
H. dried material is loaded in autoclave A7 and B8 respectively together with graphite plate, using vacuum machine 9 to height
Pressure reactor vacuumizes, after nitrogen cylinder 10 is filled with the high pressure nitrogen that purity is more than 99.99%, using the height in autoclave
Can igniter ignition reaction；
I. to particle diameter for 120-180 micron vanadium iron, reactor pressure controls in 11～12MPa, 120 points of reaction time
Clock, 1700～1800 DEG C of reaction temperature；Particle diameter is less than with 120 microns of vanadium iron, the Stress control of reactor in 8～10MPa, instead
120 minutes between seasonable, 1700～1800 DEG C of reaction temperature；
J., after reaction terminates, reactor is decompressed to normal pressure, when temperature of reaction kettle is down to below 60 DEG C, graphite plate from height
Take out in pressure reactor A and autoclave B, the iron-based vanadium nitrogen microalloy additions after sintering are separated with graphite plate；
K. the iron-based vanadium nitrogen microalloy additions after cooling are crushed with hammer mill 11, particle diameter is 10～50 millis
Rice, wherein particle diameter are less than 10 millimeters, more than 50 millimeters of footpath level sums, no more than the 6% of total amount.
Claims (2)
1. a kind of iron-based vanadium nitrogen microalloy additions it is characterised in that：By weight, 97.95 parts of 50 vanadium iron, combustion adjuvant 2.00
Part, 0.05 part of nitriding catalyst；It is prepared from by following steps：
A. 50 vanadium iron are put into broken in jaw crusher (1), be broken into the particle less than or equal to 10 millimeters；
B. broken vanadium iron particle is put in double-roll crusher (2) and pulverize further；
C. the vanadium iron after pulverizing is respectively put in ball mill (3), is ground；
D. the vanadium iron after grinding is put in vibratory sieve (4), filter out 50 vanadium iron less than or equal to 180 micron grain sizes, will be greater than
180 microns of 50 vanadium iron are reentered in ball mill (3) and continue to grind；
E. 50 vanadium iron less than or equal to 180 micron grain sizes are placed again in vibratory sieve (4), filter out 120-180 micron respectively
With two particle diameter grades less than 120 microns, classification storing；
F. different particle diameter grades are pressed, by 97.95 parts of 50 vanadium iron, 2.00 parts of combustion adjuvant aluminium powder, 0.05 part of nitriding catalyst titanium valve,
Point footpath level is attached in planet Forced Mixing machine (5), uniformly mixes；
G. the material mixing is loaded in graphite plate, put in drying machine (6) and be dried；
H. dried material is loaded in autoclave A (7) and autoclave B (8) respectively together with graphite plate, using true
Empty machine (9) vacuumizes to autoclave, after nitrogen cylinder (10) is filled with the high pressure nitrogen that purity is more than 99.99%, using height
High energy ignition unit ignition reaction in pressure reactor；
I. to particle diameter for 120-180 micron vanadium iron, reactor pressure controls in 11～12MPa, 120 minutes reaction time, instead
Answer 1700～1800 DEG C of temperature；120 microns of vanadium iron is less than to particle diameter, the Stress control of reactor in 8～10MPa, during reaction
Between 120 minutes, 1700～1800 DEG C of reaction temperature；
J., after reaction terminates, reactor is decompressed to normal pressure, when temperature of reaction kettle is down to below 60 DEG C, graphite plate is anti-from high pressure
Answer in kettle A (7) and autoclave B (8) and take out, the iron-based vanadium nitrogen microalloy additions after sintering are separated with graphite plate；
K. the iron-based vanadium nitrogen microalloy additions after cooling are crushed with hammer mill (11), particle diameter is 10～50 millis
Rice, wherein particle diameter are less than 10 millimeters, more than 50 millimeters of footpath level sums, no more than the 6% of total amount.
2. the preparation method of a kind of iron-based vanadium nitrogen microalloy additions according to claim 1, its feature takes following step
Suddenly：
A. 50 vanadium iron are put into broken in jaw crusher (1), be broken into the particle less than or equal to 10 millimeters；
B. broken vanadium iron particle is put in double-roll crusher (2) and pulverize further；
C. the vanadium iron after pulverizing is respectively put in ball mill (3), is ground；
D. the vanadium iron after grinding is put in vibratory sieve (4), filter out 50 vanadium iron less than or equal to 180 micron grain sizes, will be greater than
180 microns of 50 vanadium iron are reentered in ball mill (3) and continue to grind；
E. 50 vanadium iron less than or equal to 180 micron grain sizes are placed again in vibratory sieve (4), filter out 120-180 micron respectively
With two particle diameter grades less than 120 microns, classification storing；
F. different particle diameter grades are pressed, by 97.95 parts of 50 vanadium iron, 2.00 parts of combustion adjuvant aluminium powder, 0.05 part of nitriding catalyst titanium valve,
Point footpath level is attached in planet Forced Mixing machine (5), uniformly mixes；
G. the material mixing is loaded in graphite plate, put in drying machine (6) and be dried；
H. dried material is loaded in autoclave A (7) and autoclave B (8) respectively together with graphite plate, using true
Empty machine (9) vacuumizes to autoclave, after nitrogen cylinder (10) is filled with the high pressure nitrogen that purity is more than 99.99%, using height
High energy ignition unit ignition reaction in pressure reactor；
I. to particle diameter for 120-180 micron vanadium iron, reactor pressure controls in 11～12MPa, 120 minutes reaction time, instead
Answer 1700～1800 DEG C of temperature；120 microns of vanadium iron is less than to particle diameter, the Stress control of reactor in 8～10MPa, during reaction
Between 120 minutes, 1700～1800 DEG C of reaction temperature；
J., after reaction terminates, reactor is decompressed to normal pressure, when temperature of reaction kettle is down to below 60 DEG C, graphite plate is anti-from high pressure
Answer in kettle A (7) and autoclave B (8) and take out, the iron-based vanadium nitrogen microalloy additions after sintering are separated with graphite plate；
K. the iron-based vanadium nitrogen microalloy additions after cooling are crushed with hammer mill (11), particle diameter is 10～50 millis
Rice, wherein particle diameter are less than 10 millimeters, more than 50 millimeters of footpath level sums, no more than the 6% of total amount.
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Citations (5)
| 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 |
-
2013
- 2013-05-27 CN CN201310200028.5A patent/CN104178690B/en active Active
Patent Citations (5)
| 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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