CN108048686A - A kind of vacuum drying oven prepares ferrovanadium nitride method - Google Patents
A kind of vacuum drying oven prepares ferrovanadium nitride method Download PDFInfo
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- CN108048686A CN108048686A CN201711457346.4A CN201711457346A CN108048686A CN 108048686 A CN108048686 A CN 108048686A CN 201711457346 A CN201711457346 A CN 201711457346A CN 108048686 A CN108048686 A CN 108048686A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1078—Alloys containing non-metals by internal oxidation of material in solid state
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/16—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on nitrides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C35/00—Master alloys for iron or steel
- C22C35/005—Master alloys for iron or steel based on iron, e.g. ferro-alloys
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Abstract
The present invention relates to a kind of vacuum drying ovens to prepare ferrovanadium nitride method, it is characterized in that：Raw material is fitted into the papery mold being placed in graphite crucible, be integrally pushed into vacuum drying oven, first preheated, high temperature sintering, then passed to high pure nitrogen progress nitrogen treatment and obtain ferrovanadium nitride.Material is put into the papery mold in crucible by the present invention, is then sent directly into vacuum drying oven and is carried out nitrogen treatment, and 1）The use of binding agent is avoided in forming process, corrosion of the binding agent to vacuum drying oven is avoided, improves the service life of vacuum drying oven, while save production time and cost input；2）Crucible layer is put with layer using the mode of stacking is intersected, and preferably improves nitriding efficiency；3）Material reaction speed in vacuum drying oven is fast, and high temperature sintering temperature is low, and product yield is high, stable quality, and impurity content is low, it can be achieved that large-scale production.
Description
Technical field
The present invention relates to metallurgical technical field of smelting, and ferrovanadium nitride method is prepared more particularly to a kind of vacuum drying oven.
Background technology
Vanadium is a kind of important alloying element in steel production, its being widely used in low micro alloyed steel is general.
Research shows that vanadium is added in steel can significantly improve the intensity of steel, such as add in vanadium into steel, can make its yield strength by
350MPa is increased to more than 600MPa；Meanwhile it in steel adds vanadium can also to improve steel thermal fatigue resistance, weldability etc. comprehensive
Energy.Ferrovanadium nitride is a kind of new VN alloy additive, and performance more better than vanadium iron, more stablize, and has more by performance
The functions such as high crystal grain thinning and promotion intensity, toughness, ductility.
It is mainly produced both at home and abroad for nitrogen-containing alloy using three kinds of solid state process, liquid phase process and sintering process methods at present,
Middle solid State Nitriding, which is that one kind is common, produces vanadium alloy method, such as Chengde Branch Co., Ltd. of Hebei Iron ＆ Steel Group, uses
Ferrovanadium fine powder is put into reaction vessel, then reaction vessel feeding is prepared in stove, is passed through micro-positive pressure nitrogen, is prepared stove and is added
Heat, granular material are preparing nitriding and sintering reaction in stove, are obtaining ferrovanadium nitride product.Publication No. CN10482518A is disclosed
A kind of method that ferrovanadium nitride is prepared using vacuum drying oven, by powder vanadium and graphite, polyvinyl alcohol, iron powder is mixed in a certain ratio,
It is pressed into oblate spheroid dress material and is put into nitridation sintered in vacuum drying oven, obtained ferrovanadium nitride.The disadvantages of this method is that material need to be through two pairs of rollers
Formula pressure ball molding technique, adds production cost and process；And the water, binding agent in material have vacuum drying oven corrosion, influence
It prepares stove service life, during dry materials, generates steam, material gap is caused to increase, density is low after sintering.
The content of the invention
The purpose of the present invention is that the defects of overcoming the above-mentioned prior art, and binding agent need not be added by providing one kind, be avoided
Corrosion of the binding agent to vacuum drying oven improves service life of equipment, reduces nitriding temperature, shortens the production later stage, and realization is energy-saving,
And product quality is stablized, the low vacuum drying oven of impurity content prepares ferrovanadium nitride method.
The technical solution taken for achieving the above object is：
A kind of vacuum drying oven prepares ferrovanadium nitride method, it is characterized in that：Papery mold raw material loading being placed in graphite crucible
In, it is integrally pushed into vacuum drying oven, is first preheated, high temperature sintering, then pass to high pure nitrogen progress nitrogen treatment and obtain nitrogen
Change vanadium iron.
The graphite crucible stacks mode using intersection and is placed in vacuum drying oven.
The papery mold is handled by high temperature carbonization, thickness 8mm, specification 30*30*30mm.
Vacuum degree is between 5~20Pa in the vacuum drying oven.
The preheating refers to the temperature in vacuum furnace rising to 1000 DEG C ~ 1100 DEG C from room temperature, keeps the temperature 2~3h.
1400 DEG C~1420 DEG C of the high temperature sintering temperature, 3~4h of sintering time.
During the nitrogen treatment, 1200 DEG C~1220 DEG C, 3~4h of nitridation time of nitriding temperature is controlled, in vacuum drying oven
Nitrogen pressure is maintained at 0.02MPa.
The raw material is vanadium iron powder, wherein vanadium content 60~65%, and powder size passes through for 100 mesh 100%；
Or the combination using vanadium nitrogen powder and 50 vanadium iron powders, wherein vanadium nitrogen powder contain vanadium 75%~77%, 80 mesh 100% of granularity passes through 50 vanadium
Iron powder % containing V48~53%, the mesh of 80 mesh of granularity~100, vanadium nitrogen powder and 50 vanadium iron powder weight percent：58%~61%：38%~
41%；
Or it is combined using barium oxide, carbonaceous reducing agent and iron powder, the weight percent between three：70%~86%：5%~
15%：6%~26%.
The barium oxide is vanadium trioxide or/and vanadic anhydride, and carbonaceous reducing agent is graphite, carbon black, carburant
One or more mixing.
V 54~58%, N 11~13%, C≤0.8%, S≤0.02% in the ferrovanadium nitride, product density 5.0~
5.5g/cm3。
Material is put into the papery mold in crucible by the present invention, is then sent directly into vacuum drying oven and is carried out at nitridation
Reason, 1）The use of binding agent is avoided in forming process, corrosion of the binding agent to vacuum drying oven is avoided, improves making for vacuum drying oven
With the service life, while save production time and cost input；2）Crucible layer is put with layer using the mode of stacking is intersected, and is preferably carried
High nitriding efficiency；3）Material reaction speed in vacuum drying oven is fast, and high temperature sintering temperature is low, and product yield is high, and stable quality is miscellaneous
Matter content is low, it can be achieved that large-scale production.
Description of the drawings
Fig. 1 is papery mold and crucible schematic diagram；
Fig. 2 is crucible disposing way schematic diagram.
Specific embodiment
The present invention is explained with example, it should be understood that example is for illustrating rather than to this below
The limitation of invention.The scope of the present invention is determined with core content according to claims.
In following embodiments, papery mold is handled by high temperature carbonization, thickness 8mm.
Embodiment 1
The papery mold 2 that specification is 30*30*30mm is put into circular graphitic crucible 2, each crucible is put into 12, amounts to earthenware
Crucible number 20.By 240 kilogram of 65 vanadium iron powder, granularity is 100 mesh, is sequentially loaded into papery mold, and crucible layer intersects with layer to be stacked,
Then circular graphitic crucible is pushed into vacuum drying oven with electric flat carriage.Vacuum drying oven bell is closed, keeps sealing, vacuum degree is taken out in stove
To 5~20pa.In-furnace temperature rises to 1000 DEG C by room temperature and is kept the temperature, soaking time 1h, is continuously heating to 1420 DEG C, heat preservation
4h then passes to high pure nitrogen（N2：99.999%）, keep micro-positive pressure（0.02MPa）, in-furnace temperature is down to 1220 DEG C, carries out nitrogen
Change is handled, and nitridation time 4h, nitrogen pressure 0.02MPa are cooled to room temperature and come out of the stove, obtain ferrovanadium nitride afterwards（V：56.1%、N：
12.5%、C：0.46%, S：0.01%）, density 5.52g/cm3。
Embodiment 2
The papery mold that specification is 30*30*30mm is put into circular graphitic crucible, each crucible is put into 12, amounts to crucible
Number 20.By 150 kilograms of vanadium nitrogen powder and 90 kilograms of 50 vanadium iron powders after mixing, be packed into papery mold in, crucible layer with
Layer, which intersects, to be stacked, and then circular graphitic crucible is pushed into vacuum drying oven with electric flat carriage.Vacuum drying oven bell is closed, keeps sealing,
Vacuum degree is evacuated to 5~20pa in stove.In-furnace temperature rises to 1000 DEG C by room temperature, keeps the temperature 2h, is continuously heating to 1420 DEG C, heat preservation
3.5h then passes to high pure nitrogen（N2：99.999%）, keep micro-positive pressure（0.02MPa）, in-furnace temperature is down to 1220 DEG C, carries out
Nitrogen treatment, nitridation time 4h, nitrogen pressure 0.02MPa come out of the stove when being cooled to room temperature, obtain ferrovanadium nitride（V：54.1%、N：
11.5%、C：0.56%, S：0.01%）, density 5.34g/cm3。
Embodiment 3
The papery mold that specification is 30*30*30mm is put into circular graphitic crucible, each crucible is put into 12, amounts to crucible
Number 20.By the oxide of 160 kilograms of vanadium（Vanadium ＞ 64.7%）, 24 kilograms graphite, 56 kilograms of iron powder fills after mixing
Enter in papery mold, crucible layer intersects with layer to be stacked, and then circular graphitic crucible is pushed into vacuum drying oven with electric flat carriage.It closes
Vacuum drying oven bell keeps sealing, and vacuum degree is evacuated to 5~20pa in stove.In-furnace temperature rises to 1100 DEG C by room temperature, keeps the temperature 1.5h,
1420 DEG C are continuously heating to, 3h is kept the temperature, then passes to high pure nitrogen（N2：99.999%）, keep micro-positive pressure（0.02MPa）, in stove
Temperature is down to 1220 DEG C, carries out nitrogen treatment, nitridation time 4h, nitrogen pressure 0.02MPa come out of the stove when being cooled to room temperature, obtain
Ferrovanadium nitride（V：55%、N：10.4%、C：0.7%, S：0.02%）, density 5.40g/cm3。
Embodiment 4
The papery mold that specification is 30*30*30mm is put into circular graphitic crucible, each crucible is put into 12, amounts to crucible
Number 20.By the oxide of 150 kilograms of vanadium（Vanadium ＞ 64.7%）, 18 kilograms of graphite, 6 kilograms of carbon blacks and 66 kilograms of iron powder
It is packed into after mixing in papery mold, crucible layer intersects with layer to be stacked, and is then pushed into circular graphitic crucible with electric flat carriage
In vacuum drying oven.Vacuum drying oven bell is closed, keeps sealing, vacuum degree is evacuated to 5~20pa in stove.In-furnace temperature rises to 1100 by room temperature
DEG C, 1.5h is kept the temperature, is continuously heating to 1400 DEG C, 4h is kept the temperature, then passes to high pure nitrogen（N2：99.999%）, keep micro-positive pressure
（0.02MPa）, in-furnace temperature is down to 1220 DEG C, carries out nitrogen treatment, nitridation time 3h, nitrogen pressure 0.02MPa are cooled to room
It comes out of the stove when warm, obtains ferrovanadium nitride（V：56.1%、N：12.5%、C：0.46%, S：0.01%）, density 5.44g/cm3。
Embodiment 5
The papery mold that specification is 30*30*30mm is put into circular graphitic crucible, each crucible is put into 12, amounts to crucible
Number 20.By the oxide of 160 kilograms of vanadium（Vanadium ＞ 64.7%）, 24 kilograms carburant and 56 kilograms of iron powder after mixing
It is packed into papery mold, crucible layer intersects with layer to be stacked, and then circular graphitic crucible is pushed into vacuum drying oven with electric flat carriage.It closes
Vacuum drying oven bell is closed, keeps sealing, vacuum degree is evacuated to 5~15pa in stove.In-furnace temperature rises to 1000 DEG C by room temperature, heat preservation
1.5h is continuously heating to 1410 DEG C, keeps the temperature 4h, is passed through high pure nitrogen（N2：99.999%）, keep micro-positive pressure（0.02MPa）, stove
Interior temperature is down to 1200 DEG C, carries out nitrogen treatment, nitridation time 4h, nitrogen pressure 0.02MPa come out of the stove when being cooled to room temperature, obtain
To ferrovanadium nitride（V：58.2%、N：13.2%、C：0.39%, S：0.011%）, density 5.50g/cm3。
Claims (10)
1. a kind of vacuum drying oven prepares ferrovanadium nitride method, it is characterized in that：Raw material loading is placed in graphite crucible（1）Interior papery
Mold（2）In, it is integrally pushed into vacuum drying oven, is first preheated, high temperature sintering, then pass to high pure nitrogen and carry out nitrogen treatment
Obtain ferrovanadium nitride.
2. vacuum drying oven described in accordance with the claim 1 prepares ferrovanadium nitride method, it is characterized in that：The graphite crucible（1）Using
Intersection stacks mode and is placed in vacuum drying oven.
3. vacuum drying oven described in accordance with the claim 1 prepares ferrovanadium nitride method, it is characterized in that：The papery mold passes through high temperature
Charing process, thickness 8mm, specification 30*30*30mm.
4. vacuum drying oven described in accordance with the claim 1 prepares ferrovanadium nitride method, it is characterized in that：Vacuum degree exists in the vacuum drying oven
Between 5~20Pa.
5. vacuum drying oven described in accordance with the claim 1 prepares ferrovanadium nitride method, it is characterized in that：The preheating refers to vacuum drying oven
Interior temperature rises to 1000 DEG C ~ 1100 DEG C from room temperature, keeps the temperature 2~3h.
6. vacuum drying oven described in accordance with the claim 1 prepares ferrovanadium nitride method, it is characterized in that：The high temperature sintering temperature 1400
DEG C~1420 DEG C, 3~4h of sintering time.
7. vacuum drying oven described in accordance with the claim 1 prepares ferrovanadium nitride method, it is characterized in that：During the nitrogen treatment,
1200 DEG C~1220 DEG C of nitriding temperature is controlled, 3~4h of nitridation time, vacuum nitrogen pressure in furnace is maintained at 0.02MPa.
8. vacuum drying oven described in accordance with the claim 1 prepares ferrovanadium nitride method, it is characterized in that：The raw material is vanadium iron powder,
Middle vanadium content 60~65%, powder size pass through for 100 mesh 100%；
Or the combination using vanadium nitrogen powder and 50 vanadium iron powders, wherein vanadium nitrogen powder contain vanadium 75%~77%, 80 mesh 100% of granularity passes through 50 vanadium
Iron powder % containing V48~53%, the mesh of 80 mesh of granularity~100, vanadium nitrogen powder and 50 vanadium iron powder weight percent：58%~61%：38%~
41%；
Or it is combined using barium oxide, carbonaceous reducing agent and iron powder, the weight percent between three：70%~86%：5%~
15%：6%~26%.
9. ferrovanadium nitride method is prepared according to the vacuum drying oven described in claim 8, it is characterized in that：The barium oxide is three oxidations
Two vanadium or/and vanadic anhydride, carbonaceous reducing agent is graphite, one or more mixing of carbon black, carburant.
10. vacuum drying oven described in accordance with the claim 1 prepares ferrovanadium nitride method, it is characterized in that：V 54 in the ferrovanadium nitride
~58%, N 11~13%, C≤0.8%, S≤0.02%, 5.0~5.5g/cm of product density3。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280798A (en) * | 2018-11-28 | 2019-01-29 | 湖南众鑫新材料科技股份有限公司 | A kind of preparation method of hypoxemia VN alloy |
| CN110408884A (en) * | 2019-08-30 | 2019-11-05 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of richness nitrogen Mn-based material and preparation method thereof |
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| CN102477511A (en) * | 2010-11-30 | 2012-05-30 | 攀钢集团钢铁钒钛股份有限公司 | Method for preparing nitrided ferrovanadium |
| CN104862518A (en) * | 2015-04-21 | 2015-08-26 | 四川展祥特种合金科技有限公司 | Method for preparing nitrided ferrovanadium by using vacuum furnace |
| CN107287493A (en) * | 2017-07-05 | 2017-10-24 | 河钢股份有限公司承德分公司 | A kind of method that waste resource recovery containing vanadium is utilized |
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2017
- 2017-12-28 CN CN201711457346.4A patent/CN108048686A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102477511A (en) * | 2010-11-30 | 2012-05-30 | 攀钢集团钢铁钒钛股份有限公司 | Method for preparing nitrided ferrovanadium |
| CN104862518A (en) * | 2015-04-21 | 2015-08-26 | 四川展祥特种合金科技有限公司 | Method for preparing nitrided ferrovanadium by using vacuum furnace |
| CN107287493A (en) * | 2017-07-05 | 2017-10-24 | 河钢股份有限公司承德分公司 | A kind of method that waste resource recovery containing vanadium is utilized |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280798A (en) * | 2018-11-28 | 2019-01-29 | 湖南众鑫新材料科技股份有限公司 | A kind of preparation method of hypoxemia VN alloy |
| CN109280798B (en) * | 2018-11-28 | 2020-01-17 | 湖南众鑫新材料科技股份有限公司 | Preparation method of low-oxygen vanadium-nitrogen alloy |
| CN110408884A (en) * | 2019-08-30 | 2019-11-05 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of richness nitrogen Mn-based material and preparation method thereof |
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