CN105463515A - Method for preparing V-4Cr-4Ti alloy through fused salt electro-deoxidation method - Google Patents
Method for preparing V-4Cr-4Ti alloy through fused salt electro-deoxidation method Download PDFInfo
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
- C22C27/025—Alloys based on vanadium, niobium, or tantalum alloys based on vanadium
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Abstract
The invention discloses a method for preparing V-4Cr-4Ti alloy through a fused salt electro-deoxidation method and belongs to the fields of nonferrous metallurgy, electrochemistry and the like. The method for preparing the V-4Cr-4Ti alloy through the fused salt electro-deoxidation method comprises the following steps that (1) material mixing and tabletting are conducted, and a mixed oxide tablet is prepared through pressing after a vanadium oxide, a titanium oxide, a chrome oxide and metal powder are ball-milled and mixed according to the mass percentage; (2) the tablet is sintered, and a mixed oxide sintered body is obtained by sintering the tablet under the vacuum condition or in an inert gas atmosphere; and (3) molten salt electrolysis is conducted, electrolysis is conducted in a reactor containing a fusing electrolyte by using the mixed oxide sintered body as the cathode and using a high-purity graphite rod as the anode under the protection of inert gas, fused salt on the surface of an electrolytic product is removed, and thus the V-4Cr-4Ti alloy is obtained. According to the method for preparing the V-4Cr-4Ti alloy through the fused salt electro-deoxidation method, the technique is simple, raw materials are easy to obtain, the production cycle is short, pollution is low, the production cost is low, the current efficiency is high, and the components of prepared V-4Cr-4Ti alloy powder are uniform.
Description
Technical field
The invention belongs to the field such as Non-ferrous Metallurgy and electrochemistry, be specifically related to a kind of method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloy.
Background technology
Security is the basic premise of nuclear power development, and under high heat complicated in reactor, high radiation condition, the selection of nuclear reactor structure material is very harsh.In vanadium-base alloy, V-4Cr-4Ti alloy is due under thermodynamics complicated in fusion reactor, chemistry, stress and electromagnetic environment, there is excellent low activation characteristic, hot strength, radioprotective mutagenesis is expanded and the characteristic such as damage, good dimensional stability, high thermal conductivity, low thermal coefficient of expansion, low elastic modulus, good creep-resistant property, good processing characteristics, resistance to liquid lithium corrosion, and be considered to the excellent candidate structure material of fusion reactor of new generation.
At present, the preparation method that V-4Cr-4Ti alloy is conventional mainly contains thermit reduction, electrolytic process, vacuum melting method etc., these methods from the production and processing technology long flow path extracting alloy of raw material, pollute large, energy consumption is high, limit the application of vanadium-base alloy in every field.
It is be that raw material obtains the very low alloy etc. of foreign matter content through one-step electrolysis with oxide compound that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloy, relative to traditional preparation method, the method not only shortens technical process, decrease energy consumption and environmental pollution, reduce costs significantly, and oxide compound composition and reducing degree are easy to control.The method is the short route of V-4Cr-4Ti alloy, low cost, less energy-consumption, green metallurgical preparation open new way.Adopt the method to prepare V-4Cr-4Ti alloy hot reducing method can be avoided to introduce other impurity product purity is reduced, avoid the cyclic oxidation reduction and waste electric current between anodic-cathodic of traditional electrolyte method polyvalent metal ion, avoid adopting because of metal volatilization loss under smelting process high temperature and the uniform alloy of accurate proportioning cannot be obtained.
The ternary alloy that current employing molten salt electrodeoxidation method has been prepared mainly contains Ti-6Al-4V, Ni-35Ti-15Hf, U-40Pu-5Np etc.Consult domestic and foreign literature and also do not have the report being prepared V-4Cr-4Ti alloy by molten salt electrodeoxidation method.At present, adopting molten salt electrodeoxidation method to prepare metal and alloy, also to there is electrode conductivuty low, the problems such as in electric deoxidation process, current efficiency is low, and deoxygenation speed is low.Therefore improve the specific conductivity of electrode, the current efficiency improving reasonable offer is the problem that current this area needs to solve.
Summary of the invention
Prepare in V-4Cr-4Ti alloy process for traditional method have that energy consumption is high, the problem such as technical process length, metal volatilization loss, environmental pollution are serious, and electro-deoxiedation prepares metal and alloy, and to there is cathodic electricity conductance low, the problems such as current efficiency is low, the invention provides a kind of method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloy, prepare fusion reactor low activity structured material V-4Cr-4Ti alloy by the electro-deoxiedation improving electrolytic process current efficiency.
Molten salt electrodeoxidation method of the present invention prepares the method for V-4Cr-4Ti alloy, comprises the following steps:
Step 1, batch mixing compressing tablet:
(1) by mass percentage, barium oxide: 90 ~ 94%, titanium oxide: 2 ~ 4%, chromated oxide: 0 ~ 6%, metal powder: 0 ~ 4%, batch mixing is placed in ball grinder and mixes 2 ~ 8h, and wherein, the granularity of barium oxide, titanium oxide, chromated oxide and metal powder is 100 ~ 200 orders;
(2) by mixture, be placed in steel die and be pressed into mixed oxide compressing tablet; Wherein, forming pressure is 60 ~ 120MPa, pressurize 5 ~ 10min;
Step 2, compressing tablet sinters:
Sintered under vacuum condition or inert atmosphere by compressing tablet, sintering temperature is 1000 ~ 1200 DEG C, and sintering time 1 ~ 3h obtains mixed oxide sintered compact;
Step 3, fused salt electrolysis:
(1) using mixed oxide sintered compact as negative electrode, high purity graphite rod as anode, parallel insertion fills in the reactor of fused electrolyte carries out electrolysis, passes into protection of inert gas in electrolytic process; Wherein, electrolysis temperature is 600 ~ 900 DEG C, and electrolysis voltage is 2.8 ~ 3.1V, and electrolysis time is 2 ~ 8h;
(2) electrolysis terminates rear taking-up electrolysate, removes surperficial fused salt and obtains V-4Cr-4Ti alloy.
Wherein:
V-4Cr-4Ti alloy prepared by preparation method of the present invention, composition is Cr:3.8% ~ 4% by mass percentage, Ti:4% ~ 4.6%, and surplus is V.
In described step 1 (1), barium oxide is V
2o
3, purity>=99%; Titanium oxide is TiO
2, purity>=99%; Chromated oxide is Cr
2o
3, purity>=99%; Metal powder thing is Ti powder, purity>=99%; Add acting as of metal powder: improve electrodes conduct performance, thus improve the reactive behavior of electrode in electrolytic process;
In described step 2 and step 3, rare gas element is argon gas;
In described step 3 (1), mixed oxide sintered compact molybdenum net parcel is dressed up negative electrode with molybdenum rod Connecting groups; Ionogen is CaCl
2-NaCl mixture, is: CaCl by mass percentage
2: 67%, NaCl:33%, CaCl
2with the purity of NaCl all>=99%, granularity is 100 ~ 200 orders.
The present invention adopts barium oxide to be V
2o
3, compared with other contain barium oxide, V
2o
3have that fusing point is high, electroconductibility advantages of higher, add subject alloy component metals Ti powder simultaneously, V can be improved greatly
2o
3-Cr
2o
3-TiO
2the electroconductibility of mixed oxide electrode, is conducive to the carrying out of electrolysis, thus improves current efficiency, simultaneously newly-generated in electrolytic process metal V, and Metal Cr has higher activity, with Ti, alloying occurs under the high temperature conditions, forms V-4Cr-4Ti alloy.
Preparation technology of the present invention is simple, and raw material is easy to obtain, and with short production cycle, pollute low, production cost is low, and current efficiency is high, the V-4Cr-4Ti powdered alloy uniform composition of preparation.
Accompanying drawing explanation
The V that Fig. 1 example 1 of the present invention step 2 obtains
2o
3-Cr
2o
3-TiO
2the thing phase composite figure of mixed oxide sintered compact;
The thing phase composite figure of V-4Cr-4Ti powdered alloy prepared by Fig. 2 example 1 of the present invention;
The shape appearance figure of V-4Cr-4Ti powdered alloy prepared by Fig. 3 example 1 of the present invention.
Embodiment
In following examples, V
2o
3powder, Cr
2o
3powder, TiO
2powder, Ti powder, CaCl
2with the purity of NaCl all>=99%, granularity is 100 ~ 200 orders.
Embodiment 1
Molten salt electrodeoxidation method prepares the method for V-4Cr-4Ti alloy, comprises the following steps:
Step 1, batch mixing compressing tablet:
(1) by mass percentage, V
2o
3powder: 91.53%, Cr
2o
3powder: 3.96%, TiO
2powder: 4.51%, batch mixing is placed in ball grinder and mixes 5h;
(2) by mixture, be placed in steel die and be pressed into mixed oxide compressing tablet; Wherein, forming pressure is 100MPa, pressurize 8min; Obtaining diameter is 10mm, is highly the compressing tablet of 3mm;
Step 2, compressing tablet sinters:
Sintered under vacuum by compressing tablet, sintering temperature is 1000 DEG C, and sintering time 1h obtains mixed oxide sintered compact;
Step 3, fused salt electrolysis:
(1) mixed oxide sintered compact molybdenum net parcel is dressed up negative electrode with molybdenum rod Connecting groups, high purity graphite rod is as anode, and parallel insertion fills in the reactor of fused electrolyte carries out electrolysis, passes into argon shield in electrolytic process; Wherein, ionogen is CaCl
2-NaCl mixture, is: CaCl by mass percentage
2: 67%, NaCl:33%; Electrolysis temperature is 800 DEG C, and electrolysis voltage is 3.1V, and electrolysis time is 8h;
(2) electrolysis terminates rear taking-up electrolysate, removes surperficial fused salt and obtains V-4Cr-4Ti alloy.
The V that the present embodiment step 2 obtains
2o
3-Cr
2o
3-TiO
2the thing phase composite figure of mixed oxide sintered compact is shown in Fig. 1; The thing phase composite figure of V-4Cr-4Ti powdered alloy prepared by the present embodiment is shown in Fig. 2; The pattern of V-4Cr-4Ti powdered alloy prepared by the present embodiment is shown in Fig. 3.
The current efficiency of the present embodiment electrolysis is 48%; Each element mass content of V-4Cr-4Ti powdered alloy prepared by the present embodiment is: V91.88%, Cr3.94%, Ti4.08%.
Embodiment 2
Molten salt electrodeoxidation method prepares the method for V-4Cr-4Ti alloy, comprises the following steps:
Step 1, batch mixing compressing tablet:
(1) by mass percentage, V
2o
3powder: 92.4%, Cr
2o
3powder: 3.75%, TiO
2powder: 3.2%, Ti powder: 0.65%, batch mixing is placed in ball grinder and mixes 8h;
(2) by mixture, be placed in steel die and be pressed into mixed oxide compressing tablet; Wherein, forming pressure is 60MPa, pressurize 10min; Obtaining diameter is 10mm, is highly the compressing tablet of 3mm;
Step 2, compressing tablet sinters:
Sintered under an argon atmosphere by compressing tablet, sintering temperature is 1000 DEG C, and sintering time 3h obtains mixed oxide sintered compact;
Step 3, fused salt electrolysis:
(1) mixed oxide sintered compact molybdenum net parcel is dressed up negative electrode with molybdenum rod Connecting groups, high purity graphite rod is as anode, and parallel insertion fills in the reactor of fused electrolyte carries out electrolysis, passes into argon shield in electrolytic process; Wherein, ionogen is CaCl
2-NaCl mixture, is: CaCl by mass percentage
2: 67%, NaCl:33%; Electrolysis temperature is 600 DEG C, and electrolysis voltage is 3.0V, and electrolysis time is 4h;
(2) electrolysis terminates rear taking-up electrolysate, removes surperficial fused salt and obtains V-4Cr-4Ti alloy.
The present embodiment adds acting as of Ti powder: improve electrodes conduct performance, thus improves the reactive behavior of electrode in electrolytic process; The current efficiency of the present embodiment electrolysis is 74%; Each element mass content of V-4Cr-4Ti powdered alloy prepared by the present embodiment is:: V91.72%, Cr3.91%, Ti4.37%.
Embodiment 3
Molten salt electrodeoxidation method prepares the method for V-4Cr-4Ti alloy, comprises the following steps:
Step 1, batch mixing compressing tablet:
(1) by mass percentage, V
2o
3powder: 93.2%, Cr
2o
3powder: 4%, Ti powder: 2.8%, batch mixing is placed in ball grinder and mixes 8h;
(2) by mixture, be placed in steel die and be pressed into mixed oxide compressing tablet; Wherein, forming pressure is 100MPa, pressurize 5min; Obtaining diameter is 10mm, is highly the compressing tablet of 4mm;
Step 2, compressing tablet sinters:
Sintered under argon shield by compressing tablet, sintering temperature is 1200 DEG C, and sintering time 1h obtains mixed oxide sintered compact;
Step 3, fused salt electrolysis:
(1) mixed oxide sintered compact molybdenum net parcel is dressed up negative electrode with molybdenum rod Connecting groups, high purity graphite rod is as anode, and parallel insertion fills in the reactor of fused electrolyte carries out electrolysis, passes into argon shield in electrolytic process; Wherein, ionogen is CaCl
2-NaCl mixture, is: CaCl by mass percentage
2: 67%, NaCl:33%; Electrolysis temperature is 900 DEG C, and electrolysis voltage is 2.8V, and electrolysis time is 8h;
(2) electrolysis terminates rear taking-up electrolysate, removes surperficial fused salt and obtains V-4Cr-4Ti alloy.
The present embodiment adds acting as of Ti powder: improve electrodes conduct performance, thus improves the reactive behavior of electrode in electrolytic process; The current efficiency of the present embodiment electrolysis is 79%; Each element mass content of V-4Cr-4Ti powdered alloy prepared by the present embodiment is:: V91.78%, Cr3.82%, Ti4.4%.
Embodiment 4
Molten salt electrodeoxidation method prepares the method for V-4Cr-4Ti alloy, comprises the following steps:
Step 1, batch mixing compressing tablet:
(1) by mass percentage, V
2o
3powder: 93.2%, Cr
2o
3powder: 4%, Ti powder: 2.8%, batch mixing is placed in ball grinder and mixes 6h;
(2) by mixture, be placed in steel die and be pressed into mixed oxide compressing tablet; Wherein, forming pressure is 90MPa, pressurize 8min; Obtaining diameter is 10mm, is highly the compressing tablet of 3mm;
Step 2, compressing tablet sinters:
Sintered under vacuum by compressing tablet, sintering temperature is 1100 DEG C, and sintering time 2h obtains mixed oxide sintered compact;
Step 3, fused salt electrolysis:
(1) mixed oxide sintered compact molybdenum net parcel is dressed up negative electrode with molybdenum rod Connecting groups, high purity graphite rod is as anode, and parallel insertion fills in the reactor of fused electrolyte carries out electrolysis, passes into argon shield in electrolytic process; Wherein, ionogen is CaCl
2-NaCl mixture, is: CaCl by mass percentage
2: 67%, NaCl:33%; Electrolysis temperature is 750 DEG C, and electrolysis voltage is 3.1V, and electrolysis time is 8h;
(2) electrolysis terminates rear taking-up electrolysate, removes surperficial fused salt and obtains V-4Cr-4Ti alloy.
The present embodiment adds acting as of Ti powder: improve electrodes conduct performance, thus improves the reactive behavior of electrode in electrolytic process; The current efficiency of the present embodiment electrolysis is 69%; Each element mass content of V-4Cr-4Ti powdered alloy prepared by the present embodiment is:: V91.55%, Cr3.91%, Ti4.54%.
Embodiment 5
Molten salt electrodeoxidation method prepares the method for V-4Cr-4Ti alloy, comprises the following steps:
Step 1, batch mixing compressing tablet:
(1) by mass percentage, V
2o
3powder: 93.2%, Cr
2o
3powder: 4%, Ti powder: 2.8%, batch mixing is placed in ball grinder and mixes 7h;
(2) by mixture, be placed in steel die and be pressed into mixed oxide compressing tablet; Wherein, forming pressure is 110MPa, pressurize 7min; Obtaining diameter is 10mm, is highly the compressing tablet of 4mm;
Step 2, compressing tablet sinters:
Sintered under vacuum by compressing tablet, sintering temperature is 1050 DEG C, and sintering time 2.5h obtains mixed oxide sintered compact;
Step 3, fused salt electrolysis:
(1) mixed oxide sintered compact molybdenum net parcel is dressed up negative electrode with molybdenum rod Connecting groups, high purity graphite rod is as anode, and parallel insertion fills in the reactor of fused electrolyte carries out electrolysis, passes into argon shield in electrolytic process; Wherein, ionogen is CaCl
2-NaCl mixture, is: CaCl by mass percentage
2: 67%, NaCl:33%; Electrolysis temperature is 850 DEG C, and electrolysis voltage is 3.1V, and electrolysis time is 4h;
(2) electrolysis terminates rear taking-up electrolysate, removes surperficial fused salt and obtains V-4Cr-4Ti alloy.
The present embodiment adds acting as of Ti powder: improve electrodes conduct performance, thus improves the reactive behavior of electrode in electrolytic process; The current efficiency of the present embodiment electrolysis is 75%; Each element mass content of V-4Cr-4Ti powdered alloy prepared by the present embodiment is:: V92.11%, Cr3.82%, Ti4.07%.
Claims (6)
1. molten salt electrodeoxidation method prepares a method for V-4Cr-4Ti alloy, it is characterized in that, comprises the following steps:
Step 1, batch mixing compressing tablet:
(1) by mass percentage, barium oxide: 90 ~ 94%, titanium oxide: 2 ~ 4%, chromated oxide: 0 ~ 6%, metal powder: 0 ~ 4%, batch mixing is placed in ball grinder and mixes 2 ~ 8h, and wherein, the granularity of barium oxide, titanium oxide, chromated oxide and metal powder is 100 ~ 200 orders;
(2) by mixture, be placed in steel die and be pressed into mixed oxide compressing tablet; Wherein, forming pressure is 60 ~ 120MPa, pressurize 5 ~ 10min;
Step 2, compressing tablet sinters:
Sintered under vacuum condition or inert atmosphere by compressing tablet, sintering temperature is 1000 ~ 1200 DEG C, and sintering time 1 ~ 3h obtains mixed oxide sintered compact;
Step 3, fused salt electrolysis:
(1) using mixed oxide sintered compact as negative electrode, high purity graphite rod as anode, parallel insertion fills in the reactor of fused electrolyte carries out electrolysis, passes into protection of inert gas in electrolytic process; Wherein, electrolysis temperature is 600 ~ 900 DEG C, and electrolysis voltage is 2.8 ~ 3.1V, and electrolysis time is 2 ~ 8h;
(2) electrolysis terminates rear taking-up electrolysate, removes surperficial fused salt and obtains V-4Cr-4Ti alloy.
2. molten salt electrodeoxidation method according to claim 1 prepares the method for V-4Cr-4Ti alloy, it is characterized in that, the V-4Cr-4Ti alloy that described method is prepared, and composition is Cr:3.8% ~ 4% by mass percentage, Ti:4% ~ 4.6%, and surplus is V.
3. molten salt electrodeoxidation method according to claim 1 prepares the method for V-4Cr-4Ti alloy, it is characterized in that, in described step 1 (1), barium oxide is V
2o
3, purity>=99%; Titanium oxide is TiO
2, purity>=99%; Chromated oxide is Cr
2o
3, purity>=99%; Metal powder thing is Ti powder, purity>=99%.
4. molten salt electrodeoxidation method according to claim 1 prepares the method for V-4Cr-4Ti alloy, it is characterized in that, in described step 2 and step 3, rare gas element is argon gas.
5. molten salt electrodeoxidation method according to claim 1 prepares the method for V-4Cr-4Ti alloy, it is characterized in that, in described step 3 (1), mixed oxide sintered compact molybdenum net parcel is dressed up negative electrode with molybdenum rod Connecting groups.
6. molten salt electrodeoxidation method according to claim 1 prepares the method for V-4Cr-4Ti alloy, it is characterized in that, ionogen is CaCl
2-NaCl mixture, is: CaCl by mass percentage
2: 67%, NaCl:33%, CaCl
2with the purity of NaCl all>=99%, granularity is 100 ~ 200 orders.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107287624A (en) * | 2017-08-22 | 2017-10-24 | 攀钢集团研究院有限公司 | Prepare the process and its electrolytic cell assembly of vanadium chromium Titanium Powder |
| CN112941567A (en) * | 2018-07-10 | 2021-06-11 | 东北大学 | Electrochemical method and apparatus for high temperature molten salt electrolysis in humid atmosphere |
| CN113005481A (en) * | 2021-01-29 | 2021-06-22 | 河南大学 | Method for preparing biomedical zinc-zirconium or magnesium-zinc-zirconium alloy through electro-deoxidation |
| CN113322492A (en) * | 2021-05-28 | 2021-08-31 | 华北理工大学 | Method for preparing iron silicon from molten salt electro-deoxidation copper slag |
| CN114481228A (en) * | 2022-02-21 | 2022-05-13 | 中国工程物理研究院材料研究所 | Method for preparing uranium-titanium alloy |
| CN115449855A (en) * | 2022-10-24 | 2022-12-09 | 青岛国韬钛金属产业研究院有限公司 | Preparation method of titanium alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112941567B (en) * | 2018-07-10 | 2024-02-23 | 东北大学 | Electrochemical method and device for high-temperature molten salt electrolysis in humid atmosphere |
| CN113005481A (en) * | 2021-01-29 | 2021-06-22 | 河南大学 | Method for preparing biomedical zinc-zirconium or magnesium-zinc-zirconium alloy through electro-deoxidation |
| CN113322492A (en) * | 2021-05-28 | 2021-08-31 | 华北理工大学 | Method for preparing iron silicon from molten salt electro-deoxidation copper slag |
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| CN114481228B (en) * | 2022-02-21 | 2023-11-24 | 中国工程物理研究院材料研究所 | Method for preparing uranium titanium alloy |
| CN115449855A (en) * | 2022-10-24 | 2022-12-09 | 青岛国韬钛金属产业研究院有限公司 | Preparation method of titanium alloy |
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