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Method for preparing anti-oxidation permeated layer on surface of molybdenum or molybdenum alloy

A molybdenum alloy, anti-oxidation technology, applied in the direction of metal material coating process, coating, solid-state diffusion coating, etc., can solve the problems of insufficient oxidation resistance, fast degradation of the permeation layer, complicated preparation process, etc., to achieve Improved low-temperature oxidation resistance, quick layer deposition, and simple operation

Inactive Publication Date: 2015-08-12
CHANGAN UNIV
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Problems solved by technology

Xu et al [Acta Metallurgica Sinica,2002,15:167-171; Surface and Coatings Technology,2012,206:3393-3398] studied Al modified MoSi 2 Infiltrated layer, the infiltrated layer with Mo(Si,Al) 2 Phase-dominated, surface formed by SiO during oxidation 2 and A1 2 o 3 Composition of oxide film, compared with a single MoSi 2 The infiltrated layer shows better anti-oxidation performance, and no "pest" oxidation occurs, but the interdiffusion between the film-forming elements and the matrix in the infiltrated layer is obvious, and the infiltrated layer degrades faster
Zhang et al [International Journal of Refractory Metals and Hard Materials,2013,41:128-132] studied MoSi 2 -CrSi 2 -Si 3 N 4 Composite coating, the oxidation resistance of the composite coating is better than that of a single MoSi 2 The layer has been strengthened, but its preparation needs three times of processing, and it can be completed by step-by-step plating, and the process is complicated
In short, at present, more attention is paid to the single element modification of MoSi 2 The research on the preparation method of the infiltration layer failed to give full play to the advantages of multi-element modification, and the few multi-element modified MoSi 2 The research on the preparation method of the infiltration layer has the defects that the preparation process is complicated and the anti-oxidation performance does not meet the requirements

Method used

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  • Method for preparing anti-oxidation permeated layer on surface of molybdenum or molybdenum alloy
  • Method for preparing anti-oxidation permeated layer on surface of molybdenum or molybdenum alloy
  • Method for preparing anti-oxidation permeated layer on surface of molybdenum or molybdenum alloy

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Embodiment 1

[0026] This embodiment includes the following steps:

[0027] Step 1, polishing the surface of the molybdenum to remove the surface scale, drying after ultrasonic cleaning for 30 minutes; the molybdenum is a pure molybdenum matrix (mass purity greater than 99%);

[0028] Step 2. Prepare the embedding agent, which is made by ball milling the following raw materials in mass percentage: 12% silicon powder, 6% aluminum powder, 3% boron powder, 6% catalyst, and the balance is alumina powder body; the catalyst is ammonium fluoride powder, and the mixing time of the ball mill is 3 hours; the particle size of the silicon powder, aluminum powder, boron powder, catalyst and alumina powder is not less than 100 mesh, and the silicon powder The mass purity of aluminum powder, boron powder, catalyst and alumina powder is not less than 98%;

[0029] Step 3, embedding the dried molybdenum in step 1 in the corundum crucible containing the infiltration agent described in step 2, then sealing t...

Embodiment 2

[0041] This embodiment includes the following steps:

[0042] Step 1, polishing the surface of the molybdenum to remove the surface scale, drying after ultrasonic cleaning for 30 minutes; the molybdenum is a pure molybdenum matrix (mass purity greater than 99%);

[0043] Step 2. Prepare the osmotic agent for embedding. The osmotic agent is made by ball milling the following raw materials in mass percentage: 20% of silicon powder, 12% of aluminum powder, 4% of boron powder, 6% of catalyst, and the balance is alumina powder body; the catalyst is sodium fluoride powder, the mixing time of the ball mill is 6h; the particle size of the silicon powder, aluminum powder, boron powder, catalyst and alumina powder is not less than 100 mesh, the silicon powder The mass purity of aluminum powder, boron powder, catalyst and alumina powder is not less than 98%;

[0044] Step 3, embedding the dried molybdenum in step 1 in a graphite crucible equipped with the infiltration agent described in...

Embodiment 3

[0048] This embodiment includes the following steps:

[0049] Step 1. Grinding the surface of the molybdenum alloy to remove the surface scale, ultrasonic cleaning for 30 minutes and then drying; the molybdenum alloy is TZM molybdenum alloy;

[0050] Step 2. Prepare the embedding agent, which is made by ball milling the following raw materials in mass percentage: 12% silicon powder, 3% aluminum powder, 10% boron powder, 10% catalyst, and the balance is alumina powder body; the catalyst is ammonium chloride powder, and the mixing time of the ball mill is 5h; the particle size of the silicon powder, aluminum powder, boron powder, catalyst and alumina powder is not less than 100 mesh, and the silicon powder The mass purity of aluminum powder, boron powder, catalyst and alumina powder is not less than 98%;

[0051] Step 3, embedding the dried molybdenum alloy in step 1 in a graphite crucible filled with the infiltration agent described in step 2, then sealing the graphite crucibl...

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Abstract

The invention discloses a method for preparing an anti-oxidation permeated layer on the surface of molybdenum or a molybdenum alloy. The method comprises the following steps: I, polishing the surface of molybdenum or the molybdenum alloy so as to remove oxidized skin on the surface, performing ultrasonic washing, and drying; II, preparing a coating permeation agent; and III, coating molybdenum or the molybdenum alloy into a crucible with the permeation agent, sealing the crucible and putting the crucible into a high-temperature furnace, performing heat-preservation treatment for 1-20 hours at 1000-1500 DEG C in the presence of argon, and performing furnace cooling till the room temperature, thereby obtaining the anti-oxidation permeated layer on the surface of molybdenum or the molybdenum alloy. As the high-temperature furnace is adopted to perform heat-preservation treatment on molybdenum or the molybdenum alloy coated in the permeation agent, the anti-oxidation permeated layer of a multi-layer structure can be formed on the surface of molybdenum or the molybdenum alloy, and the anti-oxidation permeated layer is high in adaptability to the shape of a molybdenum or molybdenum alloy substrate, uniform in thickness of permeated layer, slow in degradation speed of the permeated layer, and has the advantages of simplicity in operation and rapid permeated layer deposition speed.

Description

technical field [0001] The invention belongs to the technical field of surface infiltration layer preparation, and in particular relates to a method for preparing a molybdenum or molybdenum alloy surface oxidation-resistant infiltration layer. Background technique [0002] Molybdenum-based materials (such as industrial pure molybdenum or molybdenum alloys) have the advantages of high melting point, high high-temperature strength, and moderate density. However, molybdenum is very easy to react with oxygen in an oxidizing environment above 400 °C, resulting in a significant decrease in its mechanical properties, which severely limits its use as a high-temperature structural material in a high-temperature aerobic environment. Therefore, the high-temperature resistance of molybdenum-based materials Oxidation protection is one of the key technologies to achieve its successful application at high temperature. [0003] The surface anti-oxidation coating technology is considered to...

Claims

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Application Information

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IPC IPC(8): C23C12/02
Inventor 田晓东孙志平王利捷朱施荣
Owner CHANGAN UNIV
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