Tungsten Processing - 2

Tungsten Powder
When APT is decomposed to tungsten oxides, it displays different colours according to its composition: the trioxide is yellow, the dioxide is brown, and the intermediate oxide is purple-blue. APT can be decomposed to yellow oxide when heated to above 250° C (480° F) in a furnace under a flow of air. In the industrial production of tungsten, however, APT is usually decomposed to the intermediate oxide in a rotary furnace under a stream of hydrogen, which partially decomposes the ammonia in the crystals into nitrogen and hydrogen while maintaining a reducing atmosphere. The rotary furnace is divided by partitions into three zones maintained, respectively, at 850°, 875°, and 900° C (1,550°, 1,600°, and 1,650° F). The furnace is tilted at a small angle and rotated to provide a continuous flow of powder through the central holes of the partitions.

The blue oxide is then reduced by hydrogen to metallic tungsten powder in stationary furnaces at temperatures ranging from 550° to 850° C (1,025° to 1,550° F). In this process the oxide is loaded into “boats” made of Inconel, a nickel-based alloy noted for its strength at high temperatures. These are stoked into tubes, usually arranged in two rows, and the tubes are heated in three separate zones along their lengths.

APT may also be reduced by carbon, although the powder is usually contaminated with tungsten carbide and some mineral elements contained in the carbon. When APT and carbon are mixed and reacted at 650°–850° C (1,200°–1,550° F), the product is a blue oxide. When heated in the range of 900°–1,050° C (1,650°–1,925° F), the brown oxide is formed. For complete reduction to metal, a temperature higher than 1,050° C is required. The purity of the metal is about 95 percent.

Consolidation
Tungsten powder is compacted into bars or billets with a mechanical or isostatic press prior to sintering. The “green,” or unfired, density of these compacts, obtained from powder particle sizes ranging from 1 to 10 micrometres, is usually 65 to 75 percent of the theoretical. After being presintered at 1,000°–1,200° C (1,800°–2,200° F), tungsten bars of small diameter are sintered in a hydrogen atmosphere, with heat being provided by the direct-resistance method—that is, by an electric current passed through the bar. A spring attachment to the water-cooled clips holding each bar is necessary so that one end is free to move as the bar shrinks during sintering. The current is gradually increased to raise the temperature from room temperature to 2,700°–3,100° C (4,900°–5,600° F). After holding at the final temperature for 30 to 60 minutes, the density reaches 88.5 to 96 percent of the theoretical.

An indirect sintering process is used for large tungsten billets. The heating elements of the furnace are constructed of molybdenum strips and supported by molybdenum or tungsten frames, and they are surrounded by molybdenum heat shields. A slow heating in the early stage of sintering is essential for deoxidizing the material and releasing gases at a controlled rate. At higher temperatures—i.e., from 800° C up to the final sintering temperature of 2,400° C (4,350° F)—the heating rate also should be controlled, since too fast a temperature buildup within the billet would cause thermal stresses and would result in the cracking of the material. A final sintering for 10 hours is required for densification.

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