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A kind of preparation method of refractory metal molybdenum protective film resistant to liquid lead and bismuth corrosion

A liquid lead-bismuth alloy, refractory metal technology, applied in the direction of metal material coating process, can solve the problems of corrosion, affecting material properties, poor bonding force, etc., and achieve the effect of good stability and good bonding effect

Active Publication Date: 2020-11-10
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the protection methods mainly include alloying and coating, and alloying seriously affects the original performance of the material to a large extent.
For the coating, the conventional coating method will cause problems such as poor bonding with the substrate, so allowing the structural material to react in situ in the corrosive medium to form a protective film that prevents further corrosion is currently an ideal solution to the corrosion problem.
[0007] In view of the fact that there are few reports on the corrosion protection of refractory metal molybdenum in liquid lead-bismuth, in order to solve the corrosion problem of molybdenum-based structural materials in lead-cooled fast reactors, the present invention proposes a refractory metal molybdenum protective film resistant to liquid lead-bismuth corrosion preparation method

Method used

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  • A kind of preparation method of refractory metal molybdenum protective film resistant to liquid lead and bismuth corrosion
  • A kind of preparation method of refractory metal molybdenum protective film resistant to liquid lead and bismuth corrosion
  • A kind of preparation method of refractory metal molybdenum protective film resistant to liquid lead and bismuth corrosion

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Experimental program
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Effect test

Embodiment 1

[0070] Experimental preparation process for in-situ formation of protective film of refractory metal molybdenum in liquid lead-bismuth alloy:

[0071] The refractory metal molybdenum used in this example is prepared by powder metallurgy, and its basic raw material is generally molybdenite (MoS 2 ). Molybdenum trioxide mixed with impurities can be obtained by roasting molybdenite, and then dissolving molybdenum trioxide in ammonia water to obtain ammonium paramolybdate (NH 4 ) 6 Mo 7 o 24 ) solution and filter the slag. Extract ammonium paramolybdate salt from the solution and roast at about 500°C to decompose to generate high-purity molybdenum trioxide. Molybdenum trioxide is reduced to molybdenum trioxide with hydrogen to obtain pure molybdenum powder, which is cold pressed and sintered to obtain a rod with a diameter of 90 cm, and finally extruded into a rod with a diameter of 7 mm.

[0072] The specific chemical reaction equation of the prepared molybdenum powder is a...

Embodiment 2

[0090] 1) Prepared by powder metallurgy method Molybdenum rods, and cut into two experimental samples of 3x6x50mm, remove the surface oxide skin and then carry out stress relief annealing at 900 ° C for 50 minutes; after grinding the samples with 240#, 400#, 800#, 1200#, 2000# water sandpaper , remove the scratches on the surface of the sample with a polishing cloth made of woolen material and a 2.5 μm diamond polishing agent, and finally clean it ultrasonically with alcohol for 5 minutes and dry it;

[0091] Cut the large block of lead-bismuth alloy into small pieces by cutting machine, weigh 400g to be used as corrosion medium, ultrasonically clean with alcohol for half an hour and dry;

[0092] 2) Put the weighed lead-bismuth alloy into a 50ml high-purity alumina crucible, and place it together in an atmosphere muffle furnace with a furnace temperature of 590°C for 20 minutes to completely melt the lead-bismuth alloy;

[0093] 3) Insert the sample into a crucible filled w...

Embodiment 3

[0096] 1) Prepared by powder metallurgy method Molybdenum rods, and cut into two experimental samples of 3x6x50mm, remove the surface oxide skin and then carry out stress relief annealing at 850 ° C for 60 minutes; after grinding the samples with 240#, 400#, 800#, 1200#, 2000# water sandpaper , remove the scratches on the surface of the sample with a polishing cloth made of woolen material and a 2.5 μm diamond polishing agent, and finally clean it ultrasonically with alcohol for 5 minutes and dry it;

[0097] Cut the large block of lead-bismuth alloy into small pieces by cutting machine, weigh 400g to be used as corrosion medium, ultrasonically clean with alcohol for half an hour and dry;

[0098] 2) Put the weighed lead-bismuth alloy into a 50ml high-purity alumina crucible, and place it together in an atmosphere muffle furnace with a furnace temperature of 600°C for 20 minutes to completely melt the lead-bismuth alloy;

[0099] 3) Insert the sample into a crucible filled w...

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Abstract

The invention discloses a preparation method of a refractory metal molybdenum protective film resisting liquid lead-bismuth corrosion. The preparation method comprises the steps of preparing molybdenum by a powder metallurgy method, forging, extruding and processing the molybdenum into a rod, cutting the rod into an experimental sample, and performing annealing; placing a lead-bismuth alloy in a muffle furnace to be melted into liquid lead-bismuth alloy; inserting the molybdenum rod experimental sample into a crucible containing a liquid lead-bismuth alloy, keeping the temperature and the oxygen concentration in the crucible in a saturated state, and performing corroding; cooling the liquid lead-bismuth alloy, rapidly taking out the molybdenum rod experimental sample, and placing the molybdenum rod experimental sample on a stainless steel sheet for rapid cooling; and obtaining a compact PbMoO4 / Pb2MoO5 double-layer structure metal protective film. Through detection and characterization,specific components, morphology, thickness, compactness and other comprehensive information of the protective film are obtained. The PbMoO4 / Pb2MoO5 double-layer protective film prepared by the methodgreatly prolongs the service life of the refractory metal molybdenum in the liquid lead and bismuth, and accelerates the application of the refractory metal molybdenum in the liquid lead and bismuth.

Description

technical field [0001] The invention belongs to the field of corrosion science and protection, and relates to a preparation method of a refractory metal molybdenum protective film resistant to liquid lead and bismuth corrosion. Background technique [0002] The fast neutron reactor with lead-bismuth eutectic alloy (Lead-Bismuth Eutectic, LBE) as the coolant is the lead-cooled fast reactor (LFR), which is the six main reactor types of the fourth generation reactor in the future one. In the 1950s, the basic research work of lead-cooled fast reactor was started. In 1963, the former Soviet Union successfully built the first nuclear submarine using a lead-bismuth reactor as power. After the disintegration of the Soviet Union, Russia continued to carry out civilian research and development of lead-cooled fast reactors. Currently, Russia is leading the world in lead-cooled fast reactor research. The United States and the European Union have successively carried out research and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C22/70C23C22/73
CPCC23C22/70C23C22/73
Inventor 马胜强万德才让薛德祯丁向东孙院军曾毅
Owner XI AN JIAOTONG UNIV
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