CN105463515B - A kind of method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloys - Google Patents
A kind of method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloys Download PDFInfo
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Abstract
A kind of method that molten salt electrodeoxidation method prepares V 4Cr 4Ti alloys, belongs to the fields such as non-ferrous metallurgy and electrochemistry.Include the following steps：(1) batch mixing tabletting：By barium oxide, titanium oxide, chromated oxide and metal powder, by mass percentage after ball mill mixing, it is pressed into mixed oxide tabletting；(2) tabletting is sintered：Tabletting is sintered under vacuum condition or inert atmosphere, obtains mixed oxide sintered body；(3) molten-salt electrolysis：Using mixed oxide sintered body as cathode, high purity graphite rod is as anode, under inert gas protection, is placed in the reactor for filling fused electrolyte and is electrolysed, electrolysate removes surface fused salt, obtains V 4Cr 4Ti alloys.The preparation method of the present invention, simple for process, raw material is easily obtained, with short production cycle, and pollution is low, and production cost is low, and current efficiency is high, and the V 4Cr 4Ti alloy powder ingredients of preparation are uniform.
Description
Technical field
The invention belongs to the fields such as non-ferrous metallurgy and electrochemistry, and in particular to a kind of molten salt electrodeoxidation method preparation V-
The method of 4Cr-4Ti alloys.
Background technology
Safety is the basic premise of nuclear power development, in reactor under complicated high fever, high radiation condition, nuclear reactor
The selection of structural material is very harsh.V-4Cr-4Ti alloys are due to complicated heating power in fusion reactor in vanadium-base alloy
It learns, under chemistry, stress and electromagnetic environment, expand and damage with excellent low activation characteristic, elevated temperature strength, radioresistance mutagenesis,
Good dimensional stability, high thermal conductivity, low thermal coefficient of expansion, low elastic modulus, preferable creep-resistant property, it is good plus
The characteristics such as work performance, the corrosion of resistance to liquid lithium, and it is considered as the excellent candidate structure material of fusion reactor of new generation.
Currently, the common preparation method of V-4Cr-4Ti alloys mainly has thermit reduction, electrolysis, vacuum melting method etc.,
These methods are from the production and processing technology long flow path for extracting alloy of raw material, pollution is big, high energy consumption, limit vanadium-base alloy and exist
The application of every field.
It is to obtain impurity content very through one-step electrolysis using oxide as raw material that molten salt electrodeoxidation method, which prepares V-4Cr-4Ti alloys,
Low alloy etc., relative to traditional preparation method, this method not only shortens technological process, reduces energy consumption and environment is dirty
Cost is greatly reduced in dye, and oxide composition and reducing degree are easily controllable.This method is V-4Cr-4Ti alloys
Short route, low cost, low energy consumption, green metallurgical preparation opened up a new way.Preparing V-4Cr-4Ti alloys using this method can keep away
Exempting from the other impurity of thermal reduction introducing makes product purity reduce, and avoids traditional electrolyte method polyvalent metal ion between anodic-cathodic
Cyclic oxidation restores and wastes electric current, avoids using because of metal volatilization loss under smelting process high temperature and is unable to get and accurately matches
Uniform alloy.
Mainly there are Ti-6Al-4V, Ni-35Ti-15Hf, U- using ternary alloy three-partalloy prepared by molten salt electrodeoxidation method at present
40Pu-5Np etc..Consulting domestic and foreign literature does not have the report that V-4Cr-4Ti alloys are prepared by molten salt electrodeoxidation method also.Currently,
Prepare metal and alloy using molten salt electrodeoxidation method there is also electrode conductivuties low, current efficiency is low during electro-deoxidation, deoxidation
The problems such as reaction rate is low.Therefore the conductivity of electrode is improved, it is current this field needs to improve current efficiency prepared by alloy
It solves the problems, such as.
Invention content
For in conventional method preparation V-4Cr-4Ti alloy process, there are high energy consumption, technological process length, metal volatilization damages
It loses, the problems such as environmental pollution is serious and electro-deoxiedation prepare metal and alloy there are cathode conductivity is low, and current efficiency is low etc.
Problem, the present invention provide a kind of method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloys, by improving electrolytic process electric current effect
The electro-deoxiedation of rate prepares fusion reactor low activity structural material V-4Cr-4Ti alloys.
The method that the molten salt electrodeoxidation method of the present invention prepares V-4Cr-4Ti alloys, includes the following steps：
Step 1, batch mixing tabletting：
(1) by mass percentage, barium oxide：90~94%, titanium oxide：2~4%, chromated oxide：0~6%, gold
Belong to powder：0~4%, batch mixing is placed on 2~8h of mixing in ball grinder, wherein barium oxide, titanium oxide, chromated oxide and metal
The granularity of powder is 100~200 mesh；
(2) it by mixed material, is placed in steel die and is pressed into mixed oxide tabletting；Wherein, briquetting pressure be 60~
120MPa, 5~10min of pressurize；
Step 2, tabletting is sintered：
Tabletting is sintered under vacuum condition or inert atmosphere, sintering temperature is 1000~1200 DEG C, sintering time 1~
3h obtains mixed oxide sintered body；
Step 3, molten-salt electrolysis：
(1) using mixed oxide sintered body as cathode, high purity graphite rod is inserted in parallel into as anode and fills fusion electrolysis
It is electrolysed in the reactor of matter, inert gas shielding is passed through in electrolytic process；Wherein, electrolysis temperature is 600~900 DEG C, electricity
Solution voltage is 2.8~3.1V, and electrolysis time is 2~8h；
(2) electrolysate is taken out after being electrolysed, and is removed surface fused salt and is obtained V-4Cr-4Ti alloys.
Wherein：
V-4Cr-4Ti alloys prepared by preparation method of the present invention, ingredient are Cr by mass percentage：3.8%~4%, Ti：
4%~4.6%, surplus V.
In the step 1 (1), barium oxide V2O3, purity >=99%；Titanium oxide is TiO2, purity >=99%；
Chromated oxide is Cr2O3, purity >=99%；Metal powder object is Ti powder, purity >=99%；Addition metal powder is act as：Improve electricity
Pole electric conductivity, to improve the reactivity of electrode in electrolytic process；
In the step 2 and step 3, inert gas is argon gas；
In the step 3 (1), mixed oxide sintered body is wrapped up with molybdenum net and assembles into cathode with molybdenum rod；Electricity
Solution matter is CaCl2- NaCl mixtures, by mass percentage for：CaCl2：67%, NaCl：33%, CaCl2It is equal with the purity of NaCl
>=99%, granularity is 100~200 mesh.
The present invention uses barium oxide for V2O3, compared with other are containing barium oxide, V2O3, electric conductivity height high with fusing point
The advantages that, while subject alloy component metals Ti powder is added, it can greatly improve V2O3-Cr2O3-TiO2Mixed oxide electrode
Electric conductivity, be conducive to electrolysis progress, to improve current efficiency, while metal V newly-generated in electrolytic process, metal Cr
With higher activity, alloying occurs with Ti under the high temperature conditions, forms V-4Cr-4Ti alloys.
Preparation process of the present invention is simple, and raw material is easily obtained, with short production cycle, and pollution is low, and production cost is low, current efficiency
The V-4Cr-4Ti alloy powder ingredients of height, preparation are uniform.
Description of the drawings
The V that 1 step 2 of Fig. 1 present examples obtains2O3-Cr2O3-TiO2The object phase composition figure of mixed oxide sintered body；
The object phase composition figure of V-4Cr-4Ti alloy powders prepared by Fig. 2 present examples 1；
The shape appearance figure of V-4Cr-4Ti alloy powders prepared by Fig. 3 present examples 1.
Specific implementation mode
In following embodiment, V2O3Powder, Cr2O3Powder, TiO2Powder, Ti powder, CaCl2>=99% with the purity of NaCl, granularity
It is 100~200 mesh.
Embodiment 1
The method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloys, includes the following steps：
Step 1, batch mixing tabletting：
(1) by mass percentage, V2O3Powder：91.53%, Cr2O3Powder：3.96%, TiO2Powder：4.51%, batch mixing is placed on
5h is mixed in ball grinder；
(2) it by mixed material, is placed in steel die and is pressed into mixed oxide tabletting；Wherein, briquetting pressure is
100MPa, pressurize 8min；A diameter of 10mm is obtained, is highly the tabletting of 3mm；
Step 2, tabletting is sintered：
Tabletting is sintered under vacuum, sintering temperature is 1000 DEG C, sintering time 1h, obtains mixed oxide sintering
Body；
Step 3, molten-salt electrolysis：
(1) mixed oxide sintered body is wrapped up with molybdenum net and assembles into cathode with molybdenum rod, high purity graphite rod is as sun
Pole is inserted in parallel into the reactor for fill fused electrolyte and is electrolysed, and argon gas protection is passed through in electrolytic process；Wherein, it is electrolysed
Matter is CaCl2- NaCl mixtures, by mass percentage for：CaCl2：67%, NaCl：33%；Electrolysis temperature is 800 DEG C, electrolysis
Voltage is 3.1V, electrolysis time 8h；
(2) electrolysate is taken out after being electrolysed, and is removed surface fused salt and is obtained V-4Cr-4Ti alloys.
The V that the present embodiment step 2 obtains2O3-Cr2O3-TiO2The object phase composition figure of mixed oxide sintered body is shown in Fig. 1；This
The object phase composition figure of V-4Cr-4Ti alloy powders prepared by embodiment is shown in Fig. 2；V-4Cr-4Ti alloyed powders manufactured in the present embodiment
The pattern at end is shown in Fig. 3.
The current efficiency of the present embodiment electrolysis is 48%；The each element of V-4Cr-4Ti alloy powders manufactured in the present embodiment
Mass content is：V 91.88%, Cr 3.94%, Ti 4.08%.
Embodiment 2
The method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloys, includes the following steps：
Step 1, batch mixing tabletting：
(1) by mass percentage, V2O3Powder：92.4%, Cr2O3Powder：3.75%, TiO2Powder：3.2%, Ti powder：0.65%,
Batch mixing, which is placed in ball grinder, mixes 8h；
(2) it by mixed material, is placed in steel die and is pressed into mixed oxide tabletting；Wherein, briquetting pressure is
60MPa, pressurize 10min；A diameter of 10mm is obtained, is highly the tabletting of 3mm；
Step 2, tabletting is sintered：
Tabletting is sintered under an argon atmosphere, sintering temperature is 1000 DEG C, sintering time 3h, obtains mixed oxide sintering
Body；
Step 3, molten-salt electrolysis：
(1) mixed oxide sintered body is wrapped up with molybdenum net and assembles into cathode with molybdenum rod, high purity graphite rod is as sun
Pole is inserted in parallel into the reactor for fill fused electrolyte and is electrolysed, and argon gas protection is passed through in electrolytic process；Wherein, it is electrolysed
Matter is CaCl2- NaCl mixtures, by mass percentage for：CaCl2：67%, NaCl：33%；Electrolysis temperature is 600 DEG C, electrolysis
Voltage is 3.0V, electrolysis time 4h；
(2) electrolysate is taken out after being electrolysed, and is removed surface fused salt and is obtained V-4Cr-4Ti alloys.
The present embodiment addition Ti powder is act as：Improve electrodes conduct performance, to improve the anti-of electrode in electrolytic process
Answer activity；The current efficiency of the present embodiment electrolysis is 74%；The each element matter of V-4Cr-4Ti alloy powders manufactured in the present embodiment
Measuring content is：：V 91.72%, Cr 3.91%, Ti 4.37%.
Embodiment 3
The method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloys, includes the following steps：
Step 1, batch mixing tabletting：
(1) by mass percentage, V2O3Powder：93.2%, Cr2O3Powder：4%, Ti powder：2.8%, batch mixing is placed on ball grinder
Middle mixing 8h；
(2) it by mixed material, is placed in steel die and is pressed into mixed oxide tabletting；Wherein, briquetting pressure is
100MPa, pressurize 5min；A diameter of 10mm is obtained, is highly the tabletting of 4mm；
Step 2, tabletting is sintered：
Tabletting is sintered under protection of argon gas, sintering temperature is 1200 DEG C, sintering time 1h, obtains mixed oxide sintering
Body；
Step 3, molten-salt electrolysis：
(1) mixed oxide sintered body is wrapped up with molybdenum net and assembles into cathode with molybdenum rod, high purity graphite rod is as sun
Pole is inserted in parallel into the reactor for fill fused electrolyte and is electrolysed, and argon gas protection is passed through in electrolytic process；Wherein, it is electrolysed
Matter is CaCl2- NaCl mixtures, by mass percentage for：CaCl2：67%, NaCl：33%；Electrolysis temperature is 900 DEG C, electrolysis
Voltage is 2.8V, electrolysis time 8h；
(2) electrolysate is taken out after being electrolysed, and is removed surface fused salt and is obtained V-4Cr-4Ti alloys.
The present embodiment addition Ti powder is act as：Improve electrodes conduct performance, to improve the anti-of electrode in electrolytic process
Answer activity；The current efficiency of the present embodiment electrolysis is 79%；The each element matter of V-4Cr-4Ti alloy powders manufactured in the present embodiment
Measuring content is：：V 91.78%, Cr 3.82%, Ti 4.4%.
Embodiment 4
The method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloys, includes the following steps：
Step 1, batch mixing tabletting：
(1) by mass percentage, V2O3Powder：93.2%, Cr2O3Powder：4%, Ti powder：2.8%, batch mixing is placed on ball grinder
Middle mixing 6h；
(2) it by mixed material, is placed in steel die and is pressed into mixed oxide tabletting；Wherein, briquetting pressure is
90MPa, pressurize 8min；A diameter of 10mm is obtained, is highly the tabletting of 3mm；
Step 2, tabletting is sintered：
Tabletting is sintered under vacuum, sintering temperature is 1100 DEG C, sintering time 2h, obtains mixed oxide sintering
Body；
Step 3, molten-salt electrolysis：
(1) mixed oxide sintered body is wrapped up with molybdenum net and assembles into cathode with molybdenum rod, high purity graphite rod is as sun
Pole is inserted in parallel into the reactor for fill fused electrolyte and is electrolysed, and argon gas protection is passed through in electrolytic process；Wherein, it is electrolysed
Matter is CaCl2- NaCl mixtures, by mass percentage for：CaCl2：67%, NaCl：33%；Electrolysis temperature is 750 DEG C, electrolysis
Voltage is 3.1V, electrolysis time 8h；
(2) electrolysate is taken out after being electrolysed, and is removed surface fused salt and is obtained V-4Cr-4Ti alloys.
The present embodiment addition Ti powder is act as：Improve electrodes conduct performance, to improve the anti-of electrode in electrolytic process
Answer activity；The current efficiency of the present embodiment electrolysis is 69%；The each element matter of V-4Cr-4Ti alloy powders manufactured in the present embodiment
Measuring content is：：V 91.55%, Cr 3.91%, Ti 4.54%.
Embodiment 5
The method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloys, includes the following steps：
Step 1, batch mixing tabletting：
(1) by mass percentage, V2O3Powder：93.2%, Cr2O3Powder：4%, Ti powder：2.8%, batch mixing is placed on ball grinder
Middle mixing 7h；
(2) it by mixed material, is placed in steel die and is pressed into mixed oxide tabletting；Wherein, briquetting pressure is
110MPa, pressurize 7min；A diameter of 10mm is obtained, is highly the tabletting of 4mm；
Step 2, tabletting is sintered：
Tabletting is sintered under vacuum, sintering temperature is 1050 DEG C, sintering time 2.5h, obtains mixed oxide burning
Knot body；
Step 3, molten-salt electrolysis：
(1) mixed oxide sintered body is wrapped up with molybdenum net and assembles into cathode with molybdenum rod, high purity graphite rod is as sun
Pole is inserted in parallel into the reactor for fill fused electrolyte and is electrolysed, and argon gas protection is passed through in electrolytic process；Wherein, it is electrolysed
Matter is CaCl2- NaCl mixtures, by mass percentage for：CaCl2：67%, NaCl：33%；Electrolysis temperature is 850 DEG C, electrolysis
Voltage is 3.1V, electrolysis time 4h；
(2) electrolysate is taken out after being electrolysed, and is removed surface fused salt and is obtained V-4Cr-4Ti alloys.
The present embodiment addition Ti powder is act as：Improve electrodes conduct performance, to improve the anti-of electrode in electrolytic process
Answer activity；The current efficiency of the present embodiment electrolysis is 75%；The each element matter of V-4Cr-4Ti alloy powders manufactured in the present embodiment
Measuring content is：：V 92.11%, Cr 3.82%, Ti 4.07%.
Claims (6)
1. a kind of method that molten salt electrodeoxidation method prepares V-4Cr-4Ti alloys, which is characterized in that include the following steps：
Step 1, batch mixing tabletting：
(1) by mass percentage, barium oxide：90 ~ 94%, titanium oxide：2 ~ 4%, chromated oxide：0 ~ 6%, Ti powder：0.65 ~ 4%,
Batch mixing is placed in ball grinder 2 ~ 8h of mixing, wherein barium oxide, titanium oxide, chromated oxide and Ti powder granularity be 100
~ 200 mesh；
(2) it by mixed material, is placed in steel die and is pressed into mixed oxide tabletting；Wherein, briquetting pressure be 60 ~
120MPa, 5 ~ 10min of pressurize；
Step 2, tabletting is sintered：
Tabletting is sintered under vacuum condition or inert atmosphere, sintering temperature is 1000 ~ 1200 DEG C, and 1 ~ 3h of sintering time is obtained
Mixed oxide sintered body；
Step 3, molten-salt electrolysis：
(1) using mixed oxide sintered body as cathode, high purity graphite rod is inserted in parallel into as anode and fills fused electrolyte
It is electrolysed in reactor, inert gas shielding is passed through in electrolytic process；Wherein, electrolysis temperature is 600 ~ 900 DEG C, decomposition voltage
For 2.8 ~ 3.1V, electrolysis time is 2 ~ 8h；
(2) electrolysate is taken out after being electrolysed, and is removed surface fused salt and is obtained V-4Cr-4Ti alloys.
2. the method that molten salt electrodeoxidation method according to claim 1 prepares V-4Cr-4Ti alloys, which is characterized in that described
The V-4Cr-4Ti alloys that method is prepared, ingredient are Cr by mass percentage：3.8% ~ 4%, Ti：4% ~ 4.6%, surplus V.
3. the method that molten salt electrodeoxidation method according to claim 1 prepares V-4Cr-4Ti alloys, which is characterized in that described
Step 1 (1) in, barium oxide V2O3, purity >=99%；Titanium oxide is TiO2, purity >=99%；Chromated oxide is Cr2O3,
Purity >=99%；Ti powder purity >=99%.
4. the method that molten salt electrodeoxidation method according to claim 1 prepares V-4Cr-4Ti alloys, which is characterized in that described
Step 2 and step 3 in, inert gas is argon gas.
5. the method that molten salt electrodeoxidation method according to claim 1 prepares V-4Cr-4Ti alloys, which is characterized in that described
Step 3 (1) in, by mixed oxide sintered body with molybdenum net wrap up with molybdenum rod assemble into cathode.
6. the method that molten salt electrodeoxidation method according to claim 1 prepares V-4Cr-4Ti alloys, which is characterized in that electrolysis
Matter is CaCl2- NaCl mixtures, by mass percentage for：CaCl2：67%, NaCl：33%, CaCl2With the purity of NaCl >=
99%, granularity is 100 ~ 200 mesh.
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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 |
| CN113005481B (en) * | 2021-01-29 | 2022-07-29 | 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 |
| 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 |
| CN115449855B (en) * | 2022-10-24 | 2023-07-28 | 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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| CN100532653C (en) * | 2006-11-03 | 2009-08-26 | 西北有色金属研究院 | Method for extracting titanium from electrolyzed molten salt |
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