CN104946951A - Vanadium-chromium alloy and preparation method thereof - Google Patents

Vanadium-chromium alloy and preparation method thereof Download PDF

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CN104946951A
CN104946951A CN201510402489.XA CN201510402489A CN104946951A CN 104946951 A CN104946951 A CN 104946951A CN 201510402489 A CN201510402489 A CN 201510402489A CN 104946951 A CN104946951 A CN 104946951A
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vanadium
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granularity
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CN104946951B (en
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尹丹凤
孙朝晖
陈海军
王永钢
鲜勇
余彬
王唐林
唐红建
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Abstract

The invention relates to a vanadium-chromium alloy and a preparation method thereof and belongs to the field of metallurgy. The vanadium-chromium alloy is low in cost. The vanadium-chromium alloy prepared according to the preparation method comprises 93.5%-95.5% of vanadium, 1.5%-4.5% of chromium and the balance impurity. The vanadium-chromium alloy can be used for preparation of V-4Cr-4Ti alloy. The preparation method of the vanadium-chromium alloy comprises the following steps that 1, V2O5 and Cr2O3 are used as raw materials, Ca and Mg are used as reducing agents, and Ti and TiO2 are used as regulators; 2, materials obtained in the step 1 are placed in a reaction device, and the materials are triggered to conduct a metallothermic reduction reaction through an igniter; 3, after cooling, the vanadium-chromium alloy and slag are obtained and separated, and then the vanadium-chromium alloy is obtained.

Description

A kind of vanadium Chrome metal powder and preparation method thereof
Technical field
The present invention relates to a kind of vanadium Chrome metal powder and preparation method thereof, belong to field of metallurgy.
Background technology
V-4Cr-4Ti alloy is good and become fusion nucleus reactor first wall structured material because activity is low, the thermal stresses factor is high, hot strength is high, with liquid lithium consistency, receives the concern of domestic and international many research institutions.
The method that V-4Cr-4Ti alloy is prepared in domestic and international melting mainly contains vacuum self-consumption electrode arc melting (VAR), electron beam melting (EBM) and magnetic levitation melting (LM) three kinds.Through the development of decades, adopt the ingot quality prepared of aforesaid method from a few hectogram to several kilograms not etc., even reach 1200kg, especially VAR method has become the preparation method generally adopted in the world at present, but also there is following very important shortcoming:
1) the high purity requirement of raw metal (V, Cr, Ti), adds production cost, for vanadium metal, and market value about 3,000,000 yuan/ton;
2) otherness of metal V, Cr, Ti density and fusing point makes product composition lack of homogeneity, electrode preparation difficulty and have to pass through repeated revert-melt and could improve component segregation phenomenon, complex technical process, and cost is high.
Except above-mentioned three kinds of main method, the technology that Bhabha Atomic Research Centre of India proposed aluminothermy co-reducing process prepare V-Ti-Cr alloy in 2011, this technology adopts Al to obtain V-Ti-Cr-Al-O alloy crude product as reductive agent, unnecessary Al and O is removed again by electron beam melting purification, gained alloy uniformity is good, but there is the problems such as remaining Al, experimental scale be little.
Material supply section institute of Korea S adopted C to utilize TiO as reductive agent in 2013 in laboratory 2, V 2o 5, Cr 2o 3obtain Ti, Cr, V 1.93cr 0.07o 3with VC phase, and utilize C and TiH 2, Cr and V then obtains V-Cr-Ti alloy, is also laboratory scale research.
Summary of the invention
Technical problem solved by the invention is to provide a kind of preparation method of lower-cost vanadium Chrome metal powder, and the V content of the vanadium Chrome metal powder of the method gained is 93.5 ~ 95.5, Cr content is 1.5 ~ 4.5%, and surplus is impurity; Vanadium Chrome metal powder of the present invention can be used for the crude product preparing V-4Cr-4Ti alloy, and Light absorbing impurty is required to meet the demand of preparation V-4Cr-4Ti alloy.
The preparation method of vanadium Chrome metal powder of the present invention comprises the steps:
A () is with V 2o 5, Cr 2o 3for raw material, with metal Ca, metal M g for reductive agent, with metal Ti, TiO 2for adjusting agent, mix by following weight ratio:
V 2o 5: Cr 2o 3: metal Ca: metal M g: metal Ti: TiO 2=1:0.0313 ~ 0.0355:0.547 ~ 0.588:0.287 ~ 0.295:0.187 ~ 0.233:0.787 ~ 0.832;
B step (a) gained raw material loads in conversion unit by (), cause raw material carry out metallothermic reduction reaction with priming mixture;
Obtain vanadium Chrome metal powder and slag after (c) cooling, be separated, namely obtain vanadium Chrome metal powder.
Further, in order to make vanadium Chrome metal powder impurity content meet preparation V-4Cr-4Ti requirement, the described each component of step (a) is:
Described raw material V 2o 5purity>=99.9%, and foreign matter content≤0.01% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P.
Described Cr material 2o 3purity>=99.5%, and foreign matter content≤0.05% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P.
Described reductive agent metal M g purity >=99.7%, and foreign matter content≤0.01% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P.
Described reductive agent metal Ca purity >=99.7%, and foreign matter content≤0.01% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P.
Described adjusting agent metal Ti purity >=99.5%, and foreign matter content≤0.05% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P.
Described adjusting agent TiO 2purity>=99.5%, and foreign matter content≤0.05% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P.
Adopt V 2o 5, Cr 2o 3for raw material, can directly prepare vanadium Chrome metal powder by metal-thermic, operation is simple, and cost is low.According to metal V powder and Metal Cr powder, then there is no any difference with conventional preparation techniques, with high costs; Adopt V 2o 3for raw material, then can need extra power supply not because of heat, not only cost is high, and complex process; Adopt Cr 2o 3then Cr in the oxide compound because of chromium 2o 3toxicity is low, so finally adopt V 2o 5, Cr 2o 3for raw material.
Common metal-thermic is all adopt Al to be reductive agent, metal Ca, metal M g is adopted to be that reductive agent is mainly because V-4Cr-4Ti alloy repels the existence of Al element in the inventive method, and contriver finds to adopt metal A l to be that reductive agent inevitably has the residual of Al element, high boiling point in view of Al determines it except electron beam melting purification, is difficult to its content to be reduced to less than 0.01%, and electron beam melting purification is with high costs, this has just run counter to the original intention of contriver's " low cost ".And MAGNESIUM METAL boiling point is low, can major part be removed in refining process, and the radiation of alloy can not impact, have and residual also to have no relations, therefore contriver start for adopting metal M g to be reductive agent most.But found by calculation of thermodynamics, employing MAGNESIUM METAL is reductive agent, then slag system is magnesium oxide, its fusing point is up to 2852 DEG C, must add can not increase alloy impurity composition slag former to reduce slag system fusing point, but metal fever reaction can spontaneously be carried out ensureing suitable unit furnace charge heat, so the add-on of slag former is also restricted, these two conditions must reach simultaneously just can guarantee normally carrying out of reaction, is finally determined the testing program of metal Ca, Mg coreduction by phasor, calculation of thermodynamics etc.
With metal Ti, TiO 2for adjusting agent can not only reduce the fusing point of slag system, even and if have the residual of metal Ti to be also beneficial element for vanadium Chrome metal powder, adopt Ti, TiO 2for the vanadium yield of slag system adjusting agent, at the CaO-MgO-Ti of 2200 DEG C 2o 3slag system diagram (as Fig. 1) can be found out, the slag system generated by charge composition of the present invention is melting at 2200 DEG C, and can the adiabatic combustion temperature of knowing reaction be also more than 2600 DEG C by calculation of thermodynamics, so slag, alloy can separate.
Further, if raw material granularity is excessive, then can affect metallothermic reduction speed of response, increase the reaction times, reaction also may be made insufficient, reduce the dynamic conditions of reaction; If but raw material granularity is too small, then in batch mixing, smelting process, easily cause powder to fly upward, reduce alloy yield.Therefore, the V described in step (a) 2o 5granularity is preferably 80 ~ 200 orders, Cr 2o 3granularity is preferably 80 ~ 160 orders, TiO 2granularity is preferably 120 ~ 200 orders, and metal M g granularity is preferably 3 ~ 5mm, and metal Ca granularity is preferably 3 ~ 5mm, and metal Ti granularity is preferably 3 ~ 5mm.
Further, the described conversion unit of step (b) is smelting furnace.
Further, for avoiding the impurity in furnace lining to enter, and in conjunction with MgO-CaO-Ti 2o 3slag system feature, should select electrosmelted magnesite clinker and electric molten magnesite chamotte as the knotting material of the smelting furnace furnace lining described in step (b), both purity all should>=98.5%.
Further, barium peroxide and the magnesium powder mixture of to be weight ratio the be 6.5 ~ 7.5:1 of the priming mixture described in step (b).Make priming mixture with barium peroxide and magnesium powder, exothermic oxidation amount is high, and speed of response is fast, and a small amount of reaction product formed and barium oxide and magnesium oxide can not affect slag system composition, also can not bring new impurity to alloy.
The present invention's reaction is spontaneous heat release, no matter so to be smelting temperature, time etc. be all furnace charge voluntarily exothermic heat of reaction determine, not by the control of operator, but body of heater knotting needs thicker, whole furnace chamber is tall and thin type, because can strengthen heat insulation effect like this, avoids heat radiation to reduce alloy yield too soon, and reaction terminate after can not move body of heater, at least 6 hours should be waited for just can move body of heater in order to avoid affect slag, alloy separation.
The preparation method of vanadium Chrome metal powder of the present invention, do not need to adopt pure chromium and pure vanadium to be that raw material is produced, production cost is relatively low, in gained vanadium Chrome metal powder, V content is 93.5 ~ 95.5, Cr content is 1.5 ~ 4.5%, and surplus is impurity, quality product can reach and adopt pure chromium and pure vanadium to be the quality control requirement that raw material production products obtained therefrom is suitable, can be used for preparation V-4Cr-4Ti alloy, meet industrialization need of production, have broad application prospects.
Accompanying drawing explanation
CaO during Figure 122 00 DEG C ?MgO ?Ti 2o 3phasor.
Embodiment
Now further illustrate concrete technical solution of the present invention in conjunction with the embodiments:
Embodiment 1
Get V 2o 5(purity 99.9wt%, wherein foreign matter content≤0.01% of Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P, granularity 120 ~ 160 order) 100kg, Cr 2o 3(purity 99.6wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.05% of P, granularity 80 ~ 120 order) 3.2kg, metal Ca (purity 99.8wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.01% of P, granularity 3 ~ 4mm) 55kg, metal M g (purity 99.7wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.01% of P, granularity 4 ~ 5mm) 29kg, metal Ti (purity 99.7wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.05% of P, granularity 4 ~ 5mm) 23kg, TiO 2(purity 99.5wt%, wherein foreign matter content≤0.05% of Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P, granularity 160 ~ 200 order) 83kg, the smelting furnace that electrosmelted magnesite clinker and electric molten magnesite chamotte (purity is 98.5wt%) are tied a knot is put into after they being mixed, priming mixture employing mass ratio is barium peroxide and the magnesium powder mixture of 6.8:1, adopts magnesium ribbon to ignite and cause the carrying out of main reaction as side reaction during use.After having reacted, cooling the vanadium Chrome metal powder V massfraction obtained is 95.4%, Cr massfraction 1.9%, and surplus is foreign matter content.
Embodiment 2
Get V 2o 5(purity 99.9wt%, wherein foreign matter content≤0.01% of Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P, granularity 80 ~ 120 order) 150kg, Cr 2o 3(purity 99.6wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.05% of P, granularity 120 ~ 160 order) 5kg, metal Ca (purity 99.8wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.01% of P, granularity 3 ~ 4mm) 85kg, metal M g (purity 99.7wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.01% of P, granularity 4 ~ 5mm) 45kg, metal Ti (purity 99.7wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.05% of P, granularity 3 ~ 4mm) 31kg, TiO 2(purity 99.6wt%, wherein foreign matter content≤0.05% of Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P, granularity 120 ~ 160 order) 120kg, the smelting furnace that electrosmelted magnesite clinker and electric molten magnesite chamotte (purity is 98.6wt%) are tied a knot is put into after they being mixed, priming mixture employing mass ratio is barium peroxide and the magnesium powder mixture of 7.3:1, adopts magnesium ribbon to ignite and cause the carrying out of main reaction as side reaction during use.After having reacted, cooling the vanadium Chrome metal powder V massfraction obtained is 93.8%, Cr massfraction 4.1%, and surplus is foreign matter content.
Embodiment 3
Get V 2o 5(purity 99.9wt%, wherein foreign matter content≤0.01% of Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P, granularity 160 ~ 200 order) 200kg, Cr 2o 3(purity 99.6wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.05% of P, granularity 80 ~ 120 order) 7.1kg, metal Ca (purity 99.8wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.01% of P, granularity 4 ~ 5mm) 116kg, metal M g (purity 99.7wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.01% of P, granularity 3 ~ 4mm) 59kg, metal Ti (purity 99.7wt%, wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, foreign matter content≤0.05% of P, granularity 4 ~ 5mm) 38kg, TiO 2(purity 99.6wt%, wherein foreign matter content≤0.05% of Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P, granularity 160 ~ 200 order) 158kg, the smelting furnace that electrosmelted magnesite clinker and electric molten magnesite chamotte (purity is 98.5wt%) are tied a knot is put into after they being mixed, priming mixture employing mass ratio is barium peroxide and the magnesium powder mixture of 7:1, adopts magnesium ribbon to ignite and cause the carrying out of main reaction as side reaction during use.After having reacted, cooling the vanadium Chrome metal powder V massfraction obtained is 94.5%, Cr massfraction 2.4%, and surplus is foreign matter content.
Vanadium Chrome metal powder of the present invention, in order to meet the requirement of V-4Cr-4Ti alloy, is mainly reflected in the control to foreign matter content.Known by above embodiment 1 ~ 3, gained vanadium Chrome metal powder product foreign matter content of the present invention meets the requirement of V-4Cr-4Ti alloy, and have technique simply, cost is lower, site technique workflow reengineering convenient, and feasibility is strong, the advantages such as application prospect is wide.

Claims (9)

1. the preparation method of vanadium Chrome metal powder, is characterized in that: comprise the steps:
A () is with V 2o 5, Cr 2o 3for raw material, with metal Ca, metal M g for reductive agent, with metal Ti, TiO 2for adjusting agent, mix by following weight ratio:
V 2o 5: Cr 2o 3: metal Ca: metal M g: metal Ti: TiO 2=1:0.0313 ~ 0.0355:0.547 ~ 0.588:0.287 ~ 0.295:0.187 ~ 0.233:0.787 ~ 0.832;
B step (a) gained raw material loads in conversion unit by (), cause raw material carry out metallothermic reduction reaction with priming mixture;
Obtain vanadium Chrome metal powder and slag after (c) cooling, be separated, namely obtain vanadium Chrome metal powder.
2. the preparation method of vanadium Chrome metal powder according to claim 1, is characterized in that: the described each component of step (a):
Described raw material V 2o 5purity>=99.9%, and foreign matter content≤0.01% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P;
Described Cr material 2o 3purity>=99.5%, and foreign matter content≤0.05% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P;
Described reductive agent metal M g purity >=99.7%, and foreign matter content≤0.01% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P;
Described reductive agent metal Ca purity >=99.7%, and foreign matter content≤0.01% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P;
Described adjusting agent metal Ti purity >=99.5%, and foreign matter content≤0.05% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P;
Described adjusting agent TiO 2purity>=99.5%, and foreign matter content≤0.05% of wherein Pd, Pb, Co, K, S, Bi, Ni, Mo, Nb, Cu, Al, Fe, Si, P.
3. the preparation method of vanadium Chrome metal powder according to claim 1, is characterized in that: the described each component of step (a):
Described V 2o 5granularity is 80 ~ 200 orders;
Described Cr 2o 3granularity is 80 ~ 160 orders;
Described TiO 2granularity is 120 ~ 200 orders;
Described metal M g granularity is 3 ~ 5mm;
Described metal Ca granularity is 3 ~ 5mm;
Described metal Ti granularity is 3 ~ 5mm.
4. the preparation method of vanadium Chrome metal powder according to claim 1, is characterized in that: the described conversion unit of step (b) is smelting furnace.
5. the preparation method of vanadium Chrome metal powder according to claim 4, is characterized in that: the knotting material of described smelting furnace furnace lining is at least one in electrosmelted magnesite clinker, electric molten magnesite chamotte.
6. the preparation method of vanadium Chrome metal powder according to claim 5, is characterized in that: described electrosmelted magnesite clinker, electric molten magnesite chamotte purity difference >=98.5%.
7. the preparation method of vanadium Chrome metal powder according to claim 1, is characterized in that: described priming mixture is barium peroxide and magnesium powder mixture, and its weight ratio is: barium peroxide 6.5 ~ 7.5 parts, 1 part, magnesium powder.
8. the vanadium Chrome metal powder that the preparation method described in any one of claim 1-7 prepares and obtains.
9. vanadium Chrome metal powder according to claim 8, is characterized in that: V content is 93.5 ~ 95.5, Cr content is 1.5 ~ 4.5%, and surplus is impurity.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105779841A (en) * 2015-12-28 2016-07-20 北京科技大学 Vanadium-based neutron transparent material for neutron diffraction high-pressure cavity and preparation method thereof
CN110340374A (en) * 2019-08-06 2019-10-18 攀钢集团研究院有限公司 The preparation method of vanadium chromium titanium valve
CN111957984A (en) * 2020-08-25 2020-11-20 攀钢集团攀枝花钢铁研究院有限公司 Preparation method of metal vanadium powder

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CN103320664A (en) * 2012-03-23 2013-09-25 核工业西南物理研究院 Ti3SiC2 dispersion strengthening V-4Cr-4Ti alloy
CN104561719A (en) * 2015-02-12 2015-04-29 攀钢集团攀枝花钢铁研究院有限公司 Vanadium-chromium alloy and preparation method thereof

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CN101519743A (en) * 2009-04-17 2009-09-02 攀枝花学院 Vanadium chromium aluminum alloy and method for producing the same
CN103320664A (en) * 2012-03-23 2013-09-25 核工业西南物理研究院 Ti3SiC2 dispersion strengthening V-4Cr-4Ti alloy
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CN105779841A (en) * 2015-12-28 2016-07-20 北京科技大学 Vanadium-based neutron transparent material for neutron diffraction high-pressure cavity and preparation method thereof
CN110340374A (en) * 2019-08-06 2019-10-18 攀钢集团研究院有限公司 The preparation method of vanadium chromium titanium valve
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