CN108842107A - A method of passing through sectional temperature-controlled raising VN alloy nitrogen content - Google Patents
A method of passing through sectional temperature-controlled raising VN alloy nitrogen content Download PDFInfo
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- CN108842107A CN108842107A CN201810657455.9A CN201810657455A CN108842107A CN 108842107 A CN108842107 A CN 108842107A CN 201810657455 A CN201810657455 A CN 201810657455A CN 108842107 A CN108842107 A CN 108842107A
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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
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
- C22C1/053—Making 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
- C22C1/055—Making 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C35/00—Master alloys for iron or steel
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Abstract
The present invention proposes a kind of method by sectional temperature-controlled raising VN alloy nitrogen content, includes the following steps：Ingredient mixing, green compact, body drying, sectional temperature-controlled firing and discharging, wherein sectional temperature-controlled fire includes five stages：Kiln temperature is increased to 800 DEG C by the first stage；Second stage, temperature are increased to 1200 DEG C from 800 DEG C；Phase III, temperature are increased to 1500 DEG C from 1200 DEG C；Fourth stage, temperature are stablized at 1530 DEG C；5th stage, temperature are reduced since 1530 DEG C, through forcing to be cooled within 100 DEG C.Method of the invention, it is carried out by addition nitridation promotor and to VN alloy sintering procedure sectional temperature-controlled, effectively control the reduction reaction of barium oxide, the progress of carburizing reagent and nitridation reaction, to achieve the purpose that improve VN alloy nitrogen content, the production efficiency of VN alloy is improved by the use of catalyst simultaneously, and product apparent density is made to reach 3.5g/cm3 or more.
Description
Technical field
The present invention relates to VN alloy preparation technical fields, pass through sectional temperature-controlled raising VN alloy more particularly to one kind
The method of nitrogen content.
Background technique
VN alloy is used for the production of micro alloyed steel as a kind of novel steel additive agent, alternative vanadium iron, it is added
The comprehensive mechanical performances such as the intensity, toughness, ductility and thermal fatigue resistance of steel can be improved in steel, and make steel have it is good can
Weldering property；In the case where reaching same intensity, addition VN alloy relatively addition vanadium can save vanadium 30% ~ 40%, reduce costs；VN alloy
It is generally used by domestic and international steel mill, production technology and production equipment have obtained swift and violent development.
Currently, VN alloy is produced to be restored with the oxide of vanadium with addition of reducing agent, and in all kinds of smelting furnaces
Calcining is smelted.The oxide of vanadium is usually vanadic anhydride and vanadium trioxide, by being pressed into addition of mixing after carburization agent
Type and after drying, is carbonized or nitrogenizes under the high temperature conditions and produced.The disadvantage of this method is containing for product VN alloy
Nitrogen quantity is unstable, and fluctuation is big, cannot stablize and produce the higher product of nitrogen content.
Summary of the invention
In view of the above technical problems, the object of the present invention is to provide one kind to pass through sectional temperature-controlled raising VN alloy nitrogen content
Method, this method, which passes through, to be carried out VN alloy sintering procedure sectional temperature-controlled, effectively controls the reduction reaction of barium oxide, carbon
Change reaction and the progress of nitridation reaction, to achieve the purpose that improve VN alloy nitrogen content.
To achieve the object of the present invention, a kind of method by sectional temperature-controlled raising VN alloy nitrogen content of the invention,
Include the following steps：
S1. ingredient mixes：Raw material containing barium oxide is taken, it is levigate through roller mill, reducing agent and catalyst is added, is added after dry-mixed viscous
Agent is tied, wet mixing is uniform, and nitridation promotor is added in wet mixing before terminating；
S2. green compact：The uniform material of wet mixing is subjected to pressure ball molding operation, obtains green body；
S3. body drying：By green body in the dry 10h of 200 DEG C of temperature；
S4. sectional temperature-controlled firing：Green body after drying is sent into vanadium-nitrogen alloy sintering kiln and carries out sectional temperature-controlled sintering；Segmentation
It includes five stages that temperature control, which is fired, and kiln temperature is increased to 800 DEG C by the first stage, in the temperature section with the reduction of vanadium oxide
Based on reaction；Second stage, temperature are increased to 1200 DEG C from 800 DEG C, and carburizing reagent mainly occurs in the temperature section；Third rank
Section, temperature are increased to 1500 DEG C from 1200 DEG C, sharply occur in the temperature section nitridation reaction, while carburizing reagent is still continuing；
Fourth stage, temperature are stablized at 1530 DEG C, and nitridation reaction mainly occurs in the temperature section；In 5th stage, temperature is from 1530 DEG C
Start to reduce, the material for having completed reaction starts sharply to cool down, most afterwards through forcing to be cooled within 100 DEG C；
S5. it discharges.
Preferably, the reducing agent is carbonaceous reducing agent；The catalyst is the compound of iron and iron.
Further preferably, it is 0.75 ~ 0.95% that the additional amount control of the catalyst, which is weight ratio,.
Further preferably, it is 0.8 ~ 0.85% that the additional amount control of the catalyst, which is weight ratio,
Further preferably, the catalyst is ferric carbonate.
Further preferably, the nitridation promotor is NH4HCO3。
Further preferably, in the step S4, the warm-up time of first stage is to enter tunnel from VN alloy green body
Start in kiln to 6 ~ 6.5 hours.
Further preferably, in the step S4, the warm-up time of second stage is 3 ~ 3.5 hours.
Further preferably, in the step S4, the warm-up time of phase III is 4.5 ~ 5 hours.
Further preferably, in the step S4, the temperature hold-time of fourth stage is 8 ~ 10 hours.
Compared with prior art, the method for a kind of raising VN alloy nitrogen content of the invention, by adding in the feed
Nitridation promotor is simultaneously added nitridation promotor to VN alloy sintering procedure and carries out sectional temperature-controlled, effectively controls barium oxide
Reduction reaction, carburizing reagent and nitridation reaction progress, to achieve the purpose that improve VN alloy nitrogen content, while by urging
The use of agent improves the production efficiency of VN alloy, and product apparent density is made to reach 3.5g/cm3 or more.
Detailed description of the invention
Fig. 1 is a kind of flow diagram of the method for raising VN alloy nitrogen content of the invention.
Fig. 2 is the schematic diagram of influence of the catalyst type to product density.
Fig. 3 is the schematic diagram of influence of the catalyst charge to product density.
Specific embodiment
To make to have further understanding to the purpose of the present invention, construction, feature and its function, hereby cooperate embodiment detailed
It is described as follows.
VN alloy production of new generation is using vanadic anhydride as raw material, with addition of carbonaceous reducing agent such as graphite, in nitrogen
Under protection, realized by pyroreaction.In order to improve the rate of recovery, first by V2O5VO is converted into low temperature2, V2O3, VO so as to
In control.
From the relationship analysis of barium oxide and the solid carbon free energy restored and temperature, V2O5、VO2、V2O3With the beginning of VO
The critical-temperature of reduction reaction is respectively 229.9K, 600.5K, 1464.9K and 1866.9K.Therefore barium oxide stability is suitable
Sequence is VO > V2O3> VO2> V2O5.When with V2O5When being restored for raw material, it will comply with gradually theory of reduction, i.e., change first
At VO2, then it is changed into V2O3, finally it is changed into VO.
V2O5It is converted into after the low oxide of vanadium and carries out restoring-being carbonized in kiln with solid carbon.V2O5、VO2、V2O3With
Reduction-carburizing reagent critical-temperature that starts of VO is respectively 943K, 1183K, 1377K, 1331K.When with V2O5Raw material is gone back
When former, due to V2O5Fusing point is low, volatile, therefore it need to be made as far as possible to be converted into VO during low temperature conversion2Or V2O3, then
Barium oxide is converted into vanadium carbide, then yet further carries out nitridation reaction, generates vanadium nitride.
The critical-temperature that vanadium carbide and nitrogen start nitridation reaction is 1545K.According to the property of vanadium it is found that vanadium has significantly
Carbophile and close nitrogen, that is to say, that vanadium will generate the carbide and nitride of vanadium in carbonization and nitridation process.?
1545K is hereinafter, the nitride of vanadium can be stabilized with carbide, but nitride is more more stable than carbide；Only more than 1545K
Having the carbide of vanadium can be stabilized, and the nitride of the vanadium generated at a lower temperature will the decomposition when temperature is higher than 1545K
For carbide.
Accordingly, referring to Figure 1, the method for a kind of raising VN alloy nitrogen content of one embodiment of the invention, including with
Lower step：
S1. ingredient mixes：Vanadic anhydride raw material is taken, it is levigate through roller mill, reducing agent and catalyst is added, is added after dry-mixed viscous
Agent is tied, wet mixing is uniform, and nitridation promotor is added in wet mixing before terminating；
S2. green compact：The uniform material of wet mixing is subjected to pressure ball molding operation, obtains green body；
S3. body drying：By green body in the dry 10h of 200 DEG C of temperature；
S4. sectional temperature-controlled firing：Green body after drying is sent into vanadium-nitrogen alloy sintering kiln and carries out sectional temperature-controlled sintering；
S5. it discharges.
Wherein, the sectional temperature-controlled firing in step S4 includes five stages：
First stage, VN alloy green body enter in tunnel oven to 800 DEG C, are mainly the reduction reaction of vanadium oxide in the temperature section
Based on；This stepwise heating time was since entering in tunnel oven VN alloy green body to 6 ~ 6.5 hours；
Second stage, temperature are increased to 1200 DEG C of sections from 800 DEG C, which mainly occurs carburizing reagent, while in the temperature
Section, alkali metal component such as potassium, sodium in vanadium oxide will be reduced after as gas is discharged；This stepwise heating time is 3 ~ 3.5
Hour；
Phase III, temperature are increased to 1500 DEG C from 1200 DEG C, this section of nitridation reaction sharply occurs, at the same carburizing reagent still after
It is continuous；This stepwise heating time is 4.5 ~ 5 hours；
Fourth stage, temperature are stablized at 1530 DEG C of highest, and nitridation reaction mainly occurs in the area, and the nitrogen in gas phase seeps
It penetrates into solid phase, the time used in the section is longer, is more conducive to improve the nitrogen content in product；This phase temperature duration be 8 ~
10 hours；
5th stage, temperature are reduced since 1530 DEG C, and the material for having completed reaction starts sharply to cool down, finally by forcing
It is cooled within 100 DEG C, obtains required product.
The performance of existing vanadium nitrogen alloy preparation method, reaction time length and product is poor, by using suitable catalysis
Agent can reduce reaction starting temperature, shorten the reaction time, while increasing the intensity of product.The present invention uses iron content and iron
Compound is as catalyst, first is that reaction activity can be reduced, to reduce temperature required for reaction, shortens carburizing reagent
Time；Second is that catalyst melts under the high temperature conditions, permeates in entire green body, promote the contraction of green body, significantly improve most
The density of finished product；Third is that can be used as one of the effective means of regulation product composition due to the addition of catalyst, alloy is improved
The performance of product makes V, N in product be maintained at certain ratio, while reducing the content of impurity element.
Different catalyst differs greatly to the catalytic effect of product.Fig. 2 and Fig. 3 are referred to, the present invention compared respectively
Without catalyst, catalyst A iron oxide, catalyst B ferric carbonate, influence of the catalyst C calcium oxide to product strength.Simultaneous selection
The best catalyst of effect, has done additional amount comparative test, has finally chosen with Type B catalyst ferric carbonate, additional amount control
0.8% or so（Weight percent）, properties of product can be made to reach requirement.
In a preferred embodiment of the invention, in VN alloy preparation process, in ingredient mixing, in wet mixing
Before terminating plus promotor is nitrogenized, each ingredient in green body can be made to be uniformly distributed, nitridation promotor is located at barium oxide and carbon
In the gap of matter reducing agent, VN alloy arid region and calcining kiln low-temperature space, nitridation promotor resolve into gas or
Green body is exported after gasification, during nitridation promotor leaves green body, the path that gas passes through green body forms countless microcosmic holes
Road；After reduction and carburizing reagent takes place in VN alloy green body, by the microcosmic duct formed, in a limited space
The interior diffusion flux for increasing gas is conducive to the product CO export of reaction, so that reaction balance is moved right, it is anti-to enhance reduction
It should be with the generation of carburizing reagent；After nitridation reaction takes place in VN alloy green body, the N2 of nitridation reaction is participated in by microcosmic
Duct imports inside green body, increases N2Partial pressure, enhance the generation of nitridation reaction, this manner it is also possible to significant effective improve vanadium
Nitrogen content in nitrogen alloy.In a preferred embodiment, the nitridation promotor can select NH4HCO3、(NH4)2SO4、NH4One of Cl or a variety of.
The method of a kind of raising VN alloy nitrogen content of the invention, according to vanadic anhydride by carbonaceous reducing agent mistake
The chemical reaction occurred in journey, by the way that nitridation promotor is added in the feed and carries out segmentation control to VN alloy sintering procedure
Temperature effectively controls the reduction reaction of barium oxide, the progress of carburizing reagent and nitridation reaction, contains to reach and improve VN alloy
The purpose of nitrogen quantity, while the production efficiency of VN alloy is improved by the use of preferred catalyst, and keep product apparently close
Degree reaches 3.5g/cm3 or more.
The present invention is described by above-mentioned related embodiment, however above-described embodiment is only to implement example of the invention.
It must be noted that the embodiment disclosed is not limiting as the scope of the present invention.On the contrary, do not depart from spirit of the invention and
It is changed and retouched made by range, belongs to scope of patent protection of the invention.
Claims (10)
1. a kind of pass through the sectional temperature-controlled method for improving VN alloy nitrogen content, which is characterized in that the method includes following
Step：
S1. ingredient mixes：Raw material containing barium oxide is taken, it is levigate through roller mill, reducing agent and catalyst is added, is added after dry-mixed viscous
Agent is tied, wet mixing is uniform, and nitridation promotor is added in wet mixing before terminating；
S2. green compact：The uniform material of wet mixing is subjected to pressure ball molding operation, obtains green body；
S3. body drying：By green body in the dry 10h of 200 DEG C of temperature；
S4. sectional temperature-controlled firing：Green body after drying is sent into vanadium-nitrogen alloy sintering kiln and carries out sectional temperature-controlled sintering；Segmentation
It includes five stages that temperature control, which is fired, and kiln temperature is increased to 800 DEG C by the first stage, in the temperature section with the reduction of vanadium oxide
Based on reaction；Second stage, temperature are increased to 1200 DEG C from 800 DEG C, and carburizing reagent mainly occurs in the temperature section；Third rank
Section, temperature are increased to 1500 DEG C from 1200 DEG C, sharply occur in the temperature section nitridation reaction, while carburizing reagent is still continuing；
Fourth stage, temperature are stablized at 1530 DEG C, and nitridation reaction mainly occurs in the temperature section；In 5th stage, temperature is from 1530 DEG C
Start to reduce, the material for having completed reaction starts sharply to cool down, most afterwards through forcing to be cooled within 100 DEG C；
S5. it discharges.
2. a kind of method by sectional temperature-controlled raising VN alloy nitrogen content as described in claim 1,
It is characterized in that, the reducing agent is carbonaceous reducing agent；The catalyst is the compound of iron and iron.
3. as claimed in claim 1 or 2 a kind of by the sectional temperature-controlled method for improving VN alloy nitrogen content, feature exists
In it is 0.75 ~ 0.95% that the additional amount control of the catalyst, which is weight ratio,.
4. a kind of method for passing through sectional temperature-controlled raising VN alloy nitrogen content as claimed in claim 3, which is characterized in that institute
It is 0.8 ~ 0.85% that the additional amount control for the catalyst stated, which is weight ratio,.
5. a kind of method for passing through sectional temperature-controlled raising VN alloy nitrogen content as claimed in claim 4, which is characterized in that institute
The catalyst stated is ferric carbonate.
6. a kind of method for passing through sectional temperature-controlled raising VN alloy nitrogen content as described in claim 1, which is characterized in that institute
The nitridation promotor stated is NH4HCO3。
7. a kind of method for passing through sectional temperature-controlled raising VN alloy nitrogen content as described in claim 1, which is characterized in that
In the step S4, the warm-up time of first stage was since entering in tunnel oven VN alloy green body to 6 ~ 6.5 hours.
8. a kind of method for passing through sectional temperature-controlled raising VN alloy nitrogen content as described in claim 1, which is characterized in that
In the step S4, the warm-up time of second stage is 3 ~ 3.5 hours.
9. a kind of method for passing through sectional temperature-controlled raising VN alloy nitrogen content as described in claim 1, which is characterized in that
In the step S4, the warm-up time of phase III is 4.5 ~ 5 hours.
10. a kind of method for passing through sectional temperature-controlled raising VN alloy nitrogen content as described in claim 1, which is characterized in that
In the step S4, the temperature hold-time of fourth stage is 8 ~ 10 hours.
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Cited By (2)
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| CN109694982A (en) * | 2019-03-13 | 2019-04-30 | 湖北晶洋科技股份有限公司 | The preparation process of VN alloy |
| CN114182116A (en) * | 2021-12-06 | 2022-03-15 | 江西林力高新材料有限公司 | Preparation process of low-oxygen vanadium-nitrogen alloy |
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| CN114182116A (en) * | 2021-12-06 | 2022-03-15 | 江西林力高新材料有限公司 | Preparation process of low-oxygen vanadium-nitrogen alloy |
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