CN101372321A - Method for preparing vanadium nitride - Google Patents
Method for preparing vanadium nitride Download PDFInfo
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- CN101372321A CN101372321A CNA2008100463347A CN200810046334A CN101372321A CN 101372321 A CN101372321 A CN 101372321A CN A2008100463347 A CNA2008100463347 A CN A2008100463347A CN 200810046334 A CN200810046334 A CN 200810046334A CN 101372321 A CN101372321 A CN 101372321A
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Abstract
The invention provides a method for preparing vanadium nitride. Vanadium compounds with a valence state more than four or a mixture of the compounds and organic carbon or inorganic carbon are compacted together with a binder for molding, and then the mold product is gradually heated till the temperature reaches 1,100-1,900 DEG C in a 100-4,000Hz induction heating furnace, and the product obtained is reduced and nitrified to obtain the vanadium nitride. The method has the advantages of high thermal efficiency and low power consumption.
Description
Technical field
The invention belongs to the ferrous metallurgy field, relate to the preparation method of vanadium nitride.
Background technology
Vanadium nitride is a kind of good steel-making additive, can improve and improve the comprehensive mechanical performance and the welding property of steel significantly.With use vanadium iron to compare can to save 20%～40% vanadium resource, thereby reduced the STEELMAKING PRODUCTION cost.With the construction industry is example, and the new grade III steel muscle that uses the production of VN alloy technology has not only strengthened security, shock resistance, obdurability, the welding property of buildings because of its intensity improves, and can also use regular reinforcement to save advantages such as steel 10% to 12%.
People such as J.H.Downing disclosed in US3334992 in 1967, with the V of 181Kg
2O
5, the 62Kg carbon dust, behind 4.1Kg gum resin and the 3Kg iron powder mixing, compression moulding under 20.68MPa, sample size is 51 * 51 * 38mm.Carry out carbon reduction under 1385 ℃ and 22.7Pa vacuum, system vacuum tightness drops to 2666Pa and keeps 60h again during reduction, and system vacuum tightness reverts to 22.7Pa again, indicates that promptly reduction process finishes.Stop heating with stove this moment, and sample is come out of the stove when being cooled to room temperature, and that obtain is vanadium carbide (VCx).When vacuum tightness returns to 22.7Pa, stove does not stop heating and temperature when reducing to 1100 ℃, and delivering to nitrogen in the stove and keeping the dividing potential drop of nitrogen is P
N2=700～1000Pa.The constant temperature nitriding 2h of elder generation, then furnace temperature is transferred to 1000 ℃ again nitriding 6h electric furnace stop heating, under helium-atmosphere, be chilled to room temperature and come out of the stove, the chemical constitution of its product is: 78.75%V～10.5%C～7.3%N, so claim that again this VN is VCN.
The thick grade of Wang Gong people in 1999 uses V
2O
5With the activated carbon compound stalk forming, carry out carbothermic reduction under experiment condition, reduction generates VC earlier under 1673K and 1.333Pa vacuum, feeds nitrogen subsequently, nitriding is 1.5 hours under the 101325Pa nitrogen pressure, can obtain 86%V, 7%C, 9.069%～9.577%N, 2%O sample.In order to improve vanadium nitride intensity, in raw material, add 3% iron powder.
Above-mentioned two process need condition of high vacuum degree, equipment cost and operating cost are all than higher, and do not relate to the type of heating of reaction process.
U.S. combinating carbide company disclosed in U.S. Pat 4040814 in 1977, with V
2O
3Prepared nitrogenous 12% vanadium nitride at 1100～1500 ℃ of following reduction nitridations with carbon.
People such as calendar year 2001 grandson morning sunlight disclose in Chinese patent CN1422800A; with pulverous barium oxide; briquetting behind carbonaceous pulvis and the binding agent mixing; moulding; again the material after the moulding is added the preparation stove continuously; do reaction and shielding gas to preparation stove feeding ammonia or nitrogen simultaneously; the preparation stove is heated to 1000～1800 ℃; carbonization and nitrogenizing reaction have taken place in this material in stove; time length was less than 6 hours; to under protective atmosphere, be cooled to 100～250 ℃ before coming out of the stove, come out of the stove and promptly get the vanadium nitride product.
Above-mentioned two processes are not addressed the problem of type of heating, and in fact the mode of wanting with the resistance pushed bat kiln heats.
In fact the process that discloses among above-mentioned two processes and the CN1587064 uses V
2O
3Be raw material, if use V
2O
5Be raw material, then it is not because there is a prereduction process, can melt near being its fusing point at 670 ℃ to harden, and hinders follow-up reduction process and formation product unity phenomenon.And the oxidation state of vanadium is low more in the vanadium raw materials, and raw materials cost is high more.
The people such as J.B.Goddard of Union Carbide Corporation in 1985 disclose in U.S. Pat 4562057, with the high oxide V of vanadium
2O
5Or ammonium vanadate is a raw material, with mixed gas (nitrogen+ammonia) is reductive agent and nitridizing agent, earlier at 675～700 ℃ of following prereduction 1h, low melting point high price barium oxide is reduced to dystectic low price barium oxide, under 950 ℃, reduce simultaneously afterwards and nitriding 3～4h, can obtain the product of 73.3%V, 12.6%N, 15.35%O, and then about 1400 ℃, remove wherein a large amount of oxygen with carbothermic method and get carbon vanadium nitride product.This process is through prereduction---cooling---batching---pyrocarbon thermal reduction process, and the energy consumption height, production efficiency is low, also not explanation heating in which way.
People (Thin Solid Films, 349 (1999) 14～18) such as I.Galesic had delivered with quick thermal treatment process 1100 ℃ of methods that prepare the vanadium nitride film in 1999.
2000, Prabhat Kumar Tripathy was at J.Mater.Chem., disclosed at 1500 ℃ with V in 2001,11,691～695
2O
5Be material carbon heat and N
2Reduction has prepared vanadium nitride.
Above-mentioned two processes all are the small-scale non-continuous process of research character.
The vanadium nitride preparation method who discloses in Chinese patent CN1478915A, CN2690415 is to become VO2 or V2O3 400～800 ℃ of prereduction earlier behind Vanadium Pentoxide in FLAKES and the carbon dust briquetting, finally to be reduced into vanadium nitride at 1000～1500 ℃ again.Because conductivity and magnetic property are all bad behind the mixture briquetting of barium oxide raw material and carbon dust, be difficult to heat with induction mode merely, therefore this technology adopts alloy resistance wire to heat in the mode of resistance heating in the prereduction process, is different from the present invention and all adopts induction heating in prereduction and reduction nitridation process.Though CN1757606A and CN101082089 mention the application induction furnace, do not mention the frequency of induction by current, and in patent application document and reality, all do not have actual case study on implementation.
The logical grade of Sui Zhi disclosed in Chinese patent CN1212416A in 2003, in the presence of the density reinforcer, at 1300～1500 ℃ of reduction nitridation 0.5～8h, prepared vanadium nitride.This process does not relate to the problem of adding mode, in fact finishes with resistance wire heating pushed bat kiln.
Servaas Middelhoek in 1973 etc. disclose in U.S. Pat 3745209, are raw material with the Vanadium Pentoxide in FLAKES, have synthesized vanadium nitride with ammonia and Sweet natural gas reduction nitridation down at 800～1250 ℃.Do not adopt carbothermic reduction in this process, in fact use the resistance-type rotary kiln to finish, do not mention induction heating.
Disclosing among Chinese patent CN1562770 and the CN1644510, is that raw material is preparing nitrogenous about 14% vanadium nitride more than 1420 ℃ with the method for microwave heating, with the vanadous oxide.The thermo-efficiency height of microwave heating, but because the power of single microwave tube can not be done too greatly, the general bigger power of accomplishing 5kw, so under the bigger situation of the power density that needs whole kiln, the a plurality of microwave tubes of general employing, when but microwave tube was too much, heating mutually easily between the different microwave tubes caused the reduction of microwave tube life-span, thermo-efficiency to reduce.Because microwave penetration (being generally less than 5cm) limited in one's ability, stove do can cause heating after too big inhomogeneous.More than two reasons make the single device industrial scale be restricted.General single stove is accomplished to produce per year about 100 tons of vanadium nitrides.In addition, because in the vanadium nitride preparation process, along with the intensification of reducing degree, reaction medium more and more has the character of metal, make and arrive the reaction later stage more that medium is strong more to the reflection of microwave, cause reaction to be difficult for finishing, can residual more oxygen in the product.Be different from induction heating mode of the present invention.
Zheng Chen scheme in 2002 waits in Chinese patent CN1380247A with (NH
4)
5[(VO)
6(CO
3)
4(OH)
9] 10H
2O is a raw material, has synthesized vanadium nitride under 750～1100 ℃.
People such as high Lian disclosed in Chinese patent CN1431146A in 2003, with the Vanadium Pentoxide in FLAKES (V that contains a crystal water of special methods preparation
2O
5H
2O, the crystal water mass percent is about 9%) be to prepare vanadium nitride in 3～5 hours 500～800 ℃ of insulations by raw material.
Arai in 1991, Tohru have disclosed under 700 ℃ in the metallic surface vapour deposition vanadium nitride in EP471276.
More than three kinds of methods adopt special synthetic special material, raw material obtains difficulty, price height.
Christopher Allen Bennett reached H.Kwon in its Ph D dissertation in 2002, S.Choi etc. are at Journal of Catalysis 184, disclose in the paper on 236～246 (1999), at 800～1000 ℃ of following micropreparations as the vanadium nitride of the high-specific surface area of catalyzer.The shortcoming of this method is to prepare on thermal-analysis instrumentation, and its preparation amount is very little, has only gram even milligram level.
In sum, because high price barium oxide raw material does not have electroconductibility and magnetic property poor substantially, is difficult for sensed heating, among the existing preparation method, alloy resistance wire, globars or Si-Mo rod heating element resistance heading furnace type of heating are generally adopted in all industrial mass preparations.Immediate with this patent is to adopt alloy resistance wire and the mixed type of heating heating of induction heating, adopts the resistance wire heating to be difficult for the initial feed of sensed heating in the prereduction section, treats to adopt when initial feed reverts to a certain degree induction heating again.The small scale equipment that adopts microwave heating is also arranged in addition.These resistance heating devices conduct heat slow, the thermal losses height, and the power consumption of the technology vanadium nitride per ton of resistance furnace pushed bat kiln is about 14000kWh.And microwave heating is not also maximized, and one of reduction nitridation reaction is complete inadequately.
Summary of the invention
The object of the present invention is to provide a kind of raw material to be easy to get, stable technical process is raw material with the vanadium valence state greater than the quaternary vanadium compound, heating efficiency height, the vanadium nitride production technique that energy consumption is low.
The object of the present invention is achieved like this: with oxidation state 4 valencys and vanadium compound more than 4 valencys and carbonaceous reducing agent compound stalk forming, add in the induction furnace through prereduction and reduction nitridation process generation vanadium nitride.This process is characterised in that:
The described vanadium raw materials that contains is: contain a kind of in the vanadium compound, ammonium meta-vanadate, arsenic, black vanadium, Vanadium Pentoxide in FLAKES, ammonium poly-vanadate, vanadium dioxide of the above v element of oxidation state tetravalence or tetravalence or more than one mixture, perhaps this class high price vanadium compound and the mixture that is lower than the quaternary vanadium compound;
Described heat-processed adopts induction heating, structure and processing parameter by accurately selected faradic frequency and definite induction furnace, can realize good heating to raw material, the power frequency of induction heating is 100～20000Hz, there is no need to adopt the mixed type of heating of resistive heating or microwave heating again.
Described prereduction and reduction nitridation process are carried out under 0.02～5MPa.
Described prereduction process and reduction nitridation process are finished in same reactor in turn.
Further be that described reduction nitridation process is: through the raw material of prereduction between 700～1900 ℃ by the further reduction and of inorganic carbonaceous reducing agent by the nitrogen element nitrogenize in the nitriding atmosphere, and the top temperature of material process is not less than 1100 ℃ and is not higher than 1900 ℃;
Described prereduction process and reduction nitridation process are finished in same reactor in turn, described nitriding atmosphere air-flow passes through described prereduction process again through described reduction nitridation process earlier, the heat heating that described prereduction process utilizes induction heating and gas and thermal radiation to bring from described reduction nitridation process.
Contain vanadium, nitrogen, carbon in the described vanadium nitride finished product, do not have oxygen that has reacted and the impurity of from raw material, bringing on a small quantity.
The power frequency that further is used induction heating is 100～4000Hz.The power frequency that is used for induction heating can be between 50～10MHz, and selecting the important evidence of frequency is heating efficiency and temperature.And be heated the magnetic conduction of material and the intrinsic induction power frequency of the process furnace that conductive characteristic has determined certain volume, and being higher than this frequency, whole heating systems presents the induction reactance characteristic, be lower than this frequency, present the capacitive reactance characteristic, equal this frequency, then present simple impedance characteristic.The present invention passes through the magnetic property of raw material, intermediate product and the vanadium nitride product of vanadium nitride preparation process and the research of electrical property, selected specific heat induced power frequency, this frequency makes in whole intensification and reductive process, system presents maximum impedance characteristic, make material effectively to be heated, the power-efficient height.
Further be that the induction heating furnace interior is close to solid reaction medium place the non-metallic material that one deck can sensed heating are arranged.
Further be in raw material, to add iron, ferric oxide or its mixture that is no more than vanadium weight 100% (in iron), can prepare ferruginous vanadium nitride.
Compared with the prior art, the present invention has following characteristics:
1. the selected faradic frequency of specific heating.
2. the high price barium oxide can utilize the waste heat of induction heating and reduction nitridation process to carry out prereduction, the advantage that adopts induction heating to carry out prereduction is between the piece of raw material briquetting and the piece induced electricity spark to take place easily, thereby make the carbon on piece surface and the reaction of high price barium oxide generate barium oxide at a low price, and this moment, whole temperature also was lower than 700 ℃, had avoided the fusing (fusing point of Vanadium Pentoxide in FLAKES 693 ℃) of high price barium oxide in temperature-rise period.Even be raw material with pentavalent vanadium compound or its mixture therefore, the caking or the phenomenon that hardens can not appear in whole intensification and the reduction nitridation process yet.
3. add the non-metallic material that one deck can sensed mode heats at the induction heating furnace interior near solid reaction medium place, both heating raw of induction heating like this, heat this layer of material again, conduct heat to reaction medium by this layer of material again, improve the thermo-efficiency of reaction medium under low electromagnetic induction situation.
4. prereduction and reduction nitridation process are finished in the same temperature-rise period of same reactor, have avoided independent prereduction process or have avoided adopting the higher V of price
2O
3Deng lower valency high price vanadium raw materials, energy consumption or material cost have been reduced.
Embodiment
Concrete technical solution of the present invention now is described in conjunction with the embodiments.Following examples illustrate that just technical scheme of the present invention can reliable and effectively realize, but technical solution of the present invention is not limited in following examples.
Embodiment 1
Greater than 98% piece of Vanadium, 1000kg graphite, 200kg polyethylene polyamine ball milling, briquetting is in the vertical induction kiln of packing into then with 3000kg content.The induced current frequency control is at 150Hz, the shaft kiln internal temperature in the axial direction from top to bottom by room temperature to 1500 ℃ of top temperatures, be reduced to then about 100 ℃.Block raw material adds from the shaft kiln top and continuously or intermittently from the shaft kiln bottom discharge.The shaft kiln bottom feeds nitrogen and synthetic gas (CO+H
2), reaction end gas is withdrawn from shaft kiln from the shaft kiln top.According to the output requirement, solid materials does not wait at shaft kiln internal stops 6h to 200h.Products obtained therefrom contains 78.9%V, 15.0%N, 3.1%C.Bulk product is dwindled by the raw material briquetting and is formed, no further caking phenomenon between piece and the piece.The about 5500kWh of vanadium nitride power consumption per ton.
Embodiment 2
Greater than 99% orange powdery Vanadium Pentoxide in FLAKES, 800kg gac, 200kg paraffin, 200kg starch ball milling, briquetting is in the shaft kiln of packing into then with 3000kg content.The induced current frequency control is at 2000Hz, the local liner graphite that the inner stage casing of shaft kiln contacts with the solid reaction medium, shaft kiln internal temperature in the axial direction from top to bottom by room temperature to 1500 ℃ of top temperatures, be reduced to then about 100 ℃.Block raw material adds from the shaft kiln top and continuously or intermittently from the shaft kiln bottom discharge.The shaft kiln bottom feeds nitrogen, and reaction end gas is withdrawn from shaft kiln from the shaft kiln top.According to the output requirement, solid materials does not wait at shaft kiln internal stops 6h to 200h.Products obtained therefrom contains 78.2%V, 17.3%N, 1.7%C.Bulk product is dwindled by the raw material briquetting and is formed, no further caking phenomenon between piece and the piece.The about 5000kWh of vanadium nitride power consumption per ton.
Embodiment 3
Greater than 98% piece of Vanadium, 900kg carbon black, 200kg starch ball milling, briquetting is in the shaft kiln of packing into then with 3000kg content.The induced current frequency control is at 3000Hz, the inner local liner PbO that contacts with the solid reaction medium of shaft kiln
2, the shaft kiln internal temperature in the axial direction from top to bottom by room temperature to 1300 ℃ of top temperatures, be reduced to then about 100 ℃.Block raw material adds from the shaft kiln top and continuously or intermittently from the shaft kiln bottom discharge.The shaft kiln bottom feeds nitrogen and ammonia, and reaction end gas is withdrawn from shaft kiln from the shaft kiln top.According to the output requirement, solid materials does not wait at shaft kiln internal stops 6h to 200h.Products obtained therefrom contains 77.6%V, 18.2%N, 1.1%C.Bulk product is dwindled by the raw material briquetting and is formed, no further caking phenomenon between piece and the piece.The about 4500kWh of vanadium nitride power consumption per ton.
Embodiment 4
With 3000kg content greater than 98% piece of Vanadium, 700kg graphite, 100kg starch, 100kg trimeric cyanamide ball milling, briquetting.The induced current frequency control is at 300Hz, the inner local liner carbon vanadium nitride that contacts with the solid reaction medium of pushed bat kiln, and the pushed bat kiln internal temperature, is reduced to about 100 ℃ to 1600 ℃ of top temperatures then by room temperature.Block raw material brings out material from the adding of pushed bat kiln one end and from other one continuously or intermittently with high temperature resistant uncovered magazine splendid attire.The pushed bat kiln discharge end feeds nitrogen, and the about 800 ℃ place between pushed bat kiln feed end and top temperature adds Sweet natural gas, and reaction end gas advances feed end from pushed bat kiln to be withdrawn from.According to the output requirement, solid materials does not wait at pushed bat kiln internal stops 6h to 200h.Products obtained therefrom contains 79.5%V, 12.7%N, 4.6%C.Bulk product is dwindled by the raw material briquetting and is formed, no further caking phenomenon between piece and the piece.The about 5500kWh of vanadium nitride power consumption per ton.
Embodiment 5
With 3000kg content greater than 98% piece of Vanadium, 700kg graphite, 200kg starch, 1000kg iron powder ball milling briquetting.The induced current frequency control is at 4000Hz, the mixture of local liner graphite, aluminium nitride and titanium carbonitride that the inner stage casing of pushed bat kiln contacts with the solid reaction medium, and the pushed bat kiln internal temperature, is reduced to about 100 ℃ to 1600 ℃ of top temperatures then by room temperature.Block raw material brings out material from the adding of pushed bat kiln one end and from other one continuously or intermittently with high temperature resistant uncovered magazine splendid attire.The pushed bat kiln discharge end feeds nitrogen, and the about 800 ℃ place between pushed bat kiln feed end and top temperature adds CO and H
2Mixed gas, reaction end gas advances feed end from pushed bat kiln to be withdrawn from.According to the output requirement, solid materials does not wait at pushed bat kiln internal stops 6h to 200h.Products obtained therefrom contains 32.0%Fe, 54.2%V, 8.4%N, 3.6%C.Bulk product is dwindled by the raw material briquetting and is formed, no further caking phenomenon between piece and the piece.The about 5500kWh of vanadium nitride power consumption per ton.
Claims (9)
1. the method for an industrial preparation vanadium nitride, the raw material briquetting that will contain vanadium and carbonaceous reducing agent, be heated then more than 1100 ℃, vanadium raw materials passes through prereduction process and the reduction nitridation process in nitriding atmosphere and synthetic vanadium nitride in turn in the heat-processed, it is characterized in that: the described vanadium raw materials that contains is: the vanadium compound that contains the above v element of oxidation state tetravalence or tetravalence, ammonium meta-vanadate, arsenic, black vanadium, Vanadium Pentoxide in FLAKES, ammonium poly-vanadate, a kind of in the vanadium dioxide or more than one mixture, perhaps this class high price vanadium compound and the mixture that is lower than the quaternary vanadium compound;
Described heat-processed adopts induction heating, and the power frequency of induction heating is 100～20000Hz;
Described prereduction and reduction nitridation process are carried out under 0.02～5MPa.
2. the method for preparing vanadium nitride according to claim 1 is characterized in that:
Described nitriding atmosphere is: a kind of in nitrogen, ammonia, urea, hydrazine, acetonitrile, trimeric cyanamide or other the nitrogenous organism or their mixture, the mixture of the material of perhaps above material and carbon containing or protium, the mixture of the material of perhaps above material and carbon containing and protium;
Described carbonaceous reducing agent is: a kind of in inorganic carbon, graphite, carbon black, gac, coke, refinery coke, pitch, organic carbon, starch, paraffin, the sugar or their mixture;
Described prereduction process is: above-mentioned contain in the vanadium raw materials some or all of vanadium below 700 ℃ by prereduction to the vanadium species lower than the vanadium oxidation state in the raw material;
Described reduction nitridation process is: through the raw material of prereduction between 700～1900 ℃ by the further reduction and of inorganic carbonaceous reducing agent by the nitrogen element nitrogenize in the nitriding atmosphere, and the top temperature of material process is not less than 1100 ℃ and is not higher than 1900 ℃;
Described prereduction process and reduction nitridation process are finished in same reactor in turn, described nitriding atmosphere air-flow passes through described prereduction process again through described reduction nitridation process earlier, the heat heating that described prereduction process utilizes induction heating and gas and thermal radiation to bring from described reduction nitridation process;
Contain vanadium, nitrogen, carbon in the described vanadium nitride finished product, do not have oxygen element that has reacted and the impurity of from raw material, bringing on a small quantity.
3. according to the described method for preparing vanadium nitride of arbitrary claim in the claim 1 to 2, it is characterized in that: the power frequency optimum of used induction heating is 100～4000Hz.
4. according to the described method for preparing vanadium nitride of arbitrary claim in the claim 1 to 3, it is characterized in that: the induction heating furnace interior is close to solid reaction medium place the non-metallic material that one deck can sensed heating.
5. according to the described method for preparing vanadium nitride of arbitrary claim in the claim 1 to 4, it is characterized in that: described nitriding atmosphere is the mixture of nitrogen, ammonia or above material, perhaps above material contains the mixture of reductibility hydrogen compound or the mixture of above material and CO, the mixture of perhaps above material and hydrogen and CO with hydrogen or gasiform.
6. according to the described method for preparing vanadium nitride of arbitrary claim in the claim 1 to 4, it is characterized in that: the inorganic carbonaceous reducing agent in the reduction nitridation process before the raw material briquetting with to contain vanadium raw materials mixed.
7. according to the described method for preparing vanadium nitride of arbitrary claim in the claim 1 to 4, it is characterized in that: the inorganic carbonaceous reducing agent in the reduction nitridation process is generated by organic carbonaceous reducing agent carbonization in temperature-rise period.
8. according to the described method for preparing vanadium nitride of arbitrary claim in the claim 1 to 7, it is characterized in that: in raw material, add iron, ferric oxide or its mixture that is no more than vanadium weight 100% (in iron), prepare ferruginous vanadium nitride.
9. the method for preparing vanadium nitride according to claim 4 is characterized in that: described non-metallic material contain a kind of in the oxide compound of graphite, carbon black, carbon fiber, silicon, silicon carbide, silicon nitride, aluminium nitride, plumbous oxide, ferriferous oxide, Mn oxide, chromated oxide, titanium oxide, barium oxide, vanadium nitrogen or carbide, boron or nitride or the carbide or more than one mixture and they and react the product that generates in high temperature and described nitriding atmospheres.
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| CN102785422A (en) * | 2012-08-17 | 2012-11-21 | 中国科学院宁波材料技术与工程研究所 | Vanadium nitride tool coating and manufacturing method thereof |
| CN102910596A (en) * | 2012-08-16 | 2013-02-06 | 中色（宁夏）东方集团有限公司 | Preparation method of vanadium nitride |
| CN103243254A (en) * | 2013-05-06 | 2013-08-14 | 南通汉瑞实业有限公司 | Production method of vanadium-nitrogen alloy |
| CN104404333A (en) * | 2014-11-11 | 2015-03-11 | 应忠芳 | Raw material composition for preparing vanadium nitride with ultrahigh nitrogen content and method utilizing same to prepare ultrahigh vanadium nitride |
| CN105087994A (en) * | 2015-09-06 | 2015-11-25 | 湖南众鑫新材料科技股份有限公司 | Method for preparing high-nitrogen high-purity vanadium-nitrogen alloy |
| CN106636866A (en) * | 2015-11-02 | 2017-05-10 | 陕西华银科技有限公司 | Utilization method for heat and material in vanadium-nitrogen alloy preparation |
| CN107673317A (en) * | 2017-10-27 | 2018-02-09 | 西安建筑科技大学 | A kind of method for preparing vanadium nitride |
| CN108394876A (en) * | 2017-02-07 | 2018-08-14 | 新疆晶硕新材料有限公司 | Nitrogen silane and its production method, silicon nitride and its production method |
| CN108569680A (en) * | 2018-04-23 | 2018-09-25 | 武汉科技大学 | A kind of vanadium nitride powder-body and preparation method thereof based on low temperature nitride |
| CN109536815A (en) * | 2018-11-24 | 2019-03-29 | 冯良荣 | A method of preparing nitridation manganese alloy |
| 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 |
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| CN102910596A (en) * | 2012-08-16 | 2013-02-06 | 中色（宁夏）东方集团有限公司 | Preparation method of vanadium nitride |
| CN102785422A (en) * | 2012-08-17 | 2012-11-21 | 中国科学院宁波材料技术与工程研究所 | Vanadium nitride tool coating and manufacturing method thereof |
| CN103243254A (en) * | 2013-05-06 | 2013-08-14 | 南通汉瑞实业有限公司 | Production method of vanadium-nitrogen alloy |
| CN103243254B (en) * | 2013-05-06 | 2015-05-13 | 南通汉瑞新材料科技有限公司 | Production method of vanadium-nitrogen alloy |
| CN104404333B (en) * | 2014-11-11 | 2019-01-08 | 应忠芳 | A method of it being used to prepare the feedstock composition of superelevation vanadium nitride and superelevation vanadium nitride is prepared using the raw material |
| CN104404333A (en) * | 2014-11-11 | 2015-03-11 | 应忠芳 | Raw material composition for preparing vanadium nitride with ultrahigh nitrogen content and method utilizing same to prepare ultrahigh vanadium nitride |
| CN105087994A (en) * | 2015-09-06 | 2015-11-25 | 湖南众鑫新材料科技股份有限公司 | Method for preparing high-nitrogen high-purity vanadium-nitrogen alloy |
| CN106636866A (en) * | 2015-11-02 | 2017-05-10 | 陕西华银科技有限公司 | Utilization method for heat and material in vanadium-nitrogen alloy preparation |
| CN108394876A (en) * | 2017-02-07 | 2018-08-14 | 新疆晶硕新材料有限公司 | Nitrogen silane and its production method, silicon nitride and its production method |
| CN107673317A (en) * | 2017-10-27 | 2018-02-09 | 西安建筑科技大学 | A kind of method for preparing vanadium nitride |
| CN108569680A (en) * | 2018-04-23 | 2018-09-25 | 武汉科技大学 | A kind of vanadium nitride powder-body and preparation method thereof based on low temperature nitride |
| CN109536815A (en) * | 2018-11-24 | 2019-03-29 | 冯良荣 | A method of preparing nitridation manganese alloy |
| 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 |
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