Preparation of nano rare-earth oxide doping molybdenum alloys

A technology of rare earth oxides and nano-rare earths, which is applied in the field of preparation of nano-scale rare earth oxide-doped molybdenum alloy materials. Improved strength and fracture toughness, excellent deep processing performance, and improved deformation processing

Inactive Publication Date: 2010-06-23
临沂明华管业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current traditional preparation technology of doped molybdenum alloy is difficult to meet this demand.
[0004] Currently, there are three commonly used preparation methods for oxide-doped molybdenum alloys: solid-solid doping method, liquid-solid doping method and liquid-liquid doping method. Among them, the solid-solid doping method has the advantages of simple operation and easy industrialization. The uniformity of the doped rare earth oxide distribution is poor and it is easy to bring in impurity elements, which leads to the failure of the performance of the prepared molybdenum material to meet the ideal requirements.
The liquid-solid doping method is currently widely used in industrial production. Although the uniformity of phase dispersion has been greatly improved, the degree of uniformity is still not ideal, especially the size of rare earth oxides is difficult to control. The refinement of alloy grains is not obvious and it is difficult to avoid the introduction of interstitial impurity elements, so it is difficult to obtain high-performance molybdenum alloy materials
Molybdenum alloy obtained by liquid-liquid doping method has the best effect of uniform distribution of doped second-phase particles. The process is complicated, and the size of the second phase particles in the obtained molybdenum alloy products is difficult to control, which is basically on the order of microns, and it is difficult to obtain evenly distributed nano-scale second phase particles, which limits the preparation of high-performance molybdenum alloy materials. Technological breakthroughs have restricted the development and wide application of high value-added molybdenum alloy deep-processing products that are urgently needed by the market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 5000 grams of rare earth ammonium dimolybdate powder containing 0.3wt% lanthanum oxide, roast and reduce for a period of time at 390°C for 1.2 hours, and pass hydrogen protection during the process. The pressure of the hydrogen flow is 0.3Pa, and the flow rate is 0.5m 3 / h, and then reduce at 930°C, the reduction time is 2h, the pressure of hydrogen in the reduction process is 0.3Pa, and the flow rate is 1.0m 3 / h. The reduced molybdenum alloy powder is sieved through a 160-mesh sieve, and the finished product rate reaches 99.2%. The sieved molybdenum alloy powder was cold isostatically pressed at 190 MPa for 15 min, and the formed billet was pre-sintered in a muffle furnace at a sintering temperature of 1180 ° C for 1 h. Sintered in a vacuum intermediate frequency induction sintering furnace, the sintering temperature is 1700°C, and the sintering time is 15 hours. The sintered billet is rolled by a walking mill to obtain a molybdenum alloy rod with a total def...

Embodiment 2

[0027] Weigh 5000 grams of rare earth ammonium dimolybdate powder containing 0.6wt% lanthanum oxide, roast and reduce for a period of time at 420 ° C for 1.0 h, pass hydrogen protection during the process, the pressure of the hydrogen flow is 0.3 Pa, and the flow rate is 0.5m 3 / h, and then reduce at 950°C, the reduction time is 2.5h, the pressure of hydrogen in the reduction process is 0.3Pa, and the flow rate is 1.2m 3 / h. The reduced molybdenum alloy powder is sieved through a 160-mesh sieve, and the finished product rate reaches 99.1%. The sieved molybdenum alloy powder was cold isostatically pressed at 200 MPa for 15 min, and the formed billet was pre-sintered in a muffle furnace at a sintering temperature of 1150 ° C for 1 h. Sintered in a vacuum intermediate frequency induction sintering furnace, the sintering temperature is 1600°C, and the sintering time is 18 hours. The sintered billet is rolled by a walking mill to obtain a molybdenum alloy rod with a total deform...

Embodiment 3

[0029] Weigh 5000 grams of rare earth ammonium dimolybdate powder containing 0.9wt% lanthanum oxide, roast and reduce for a period of time at 450 ° C for 1.0 h, pass hydrogen protection during the process, the pressure of the hydrogen flow is 0.3 Pa, and the flow rate is 0.4m 3 / h, and then reduce at 960°C, the reduction time is 2.5h, the pressure of the hydrogen in the reduction process is 0.3Pa, and the flow rate is 1.1m 3 / h. The reduced molybdenum alloy powder is sieved through a 160-mesh sieve, and the finished product rate reaches 99.2%. The sieved molybdenum alloy powder is cold isostatically pressed at 200 MPa for 20 minutes, and the formed blank is pre-sintered in a muffle furnace at a sintering temperature of 1200 °C for 1.2 hours. Sintered in a vacuum intermediate frequency induction sintering furnace, the sintering temperature is 1780°C, and the sintering time is 16 hours. The sintered billet is rolled by a walking mill to obtain a molybdenum alloy rod with a tot...

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Abstract

The invention discloses a method for preparing a nano rare earth oxide doped molybdenum alloy. In the method, by taking rare earth ammonium dimolybdate crystals as raw materials and adopting the roasting and hydrogen reduction method, molybdenum alloy powder is obtained, the powder after reduction is in press-forming by the isostatic cool pressing with a pressure of between 180 and 200 Mpa, the formed blank materials are presintered in a muffle furnace with a temperature of between 1, 100 and 1, 300 DEG C, and sintered in a vacuum intermediate frequency induction sintering furnace at a temperature of between 1, 600 and 1, 900 DEG C for 10 to 24 hours; the materials sintered can be made by the prior mechanical processing methods into materials and products with different shape such as molybdenum alloy bar materials or plate materials, etc. as required. The molybdenum alloy containing nano rare earth oxide, prepared by the method of the invention, has the advantages of high intensity, ductility and toughness and wide application.

Description

technical field [0001] The invention relates to a preparation method of a rare earth oxide doped molybdenum alloy material, in particular to a preparation method of a nanoscale rare earth oxide doped molybdenum alloy material. Background technique [0002] Molybdenum metal materials do not have the property of crystallographic phase transition due to temperature changes, but have the intrinsic characteristics of ductile-brittle transition and low-temperature brittleness inherent in body-centered cubic metals. Therefore, how to further improve the toughness of molybdenum metal materials to improve their machinability has become the key to the development of molybdenum metal deep-processing products and to expand their application fields! In the late 1980s, Japan, Germany, Austria, China and other countries almost simultaneously started the research on molybdenum alloys with rare earth oxide liquid-solid doping (rare earth nitrate solution sprayed in solid molybdenum oxide pow...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22C1/04B22F9/20C22F1/18
Inventor 孙军张国君孙院军刘刚江峰丁向东
Owner 临沂明华管业有限公司
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