Abstract
The objective of this research project is to produce single crystal niobium (Nb) tubes for use as particle accelerator cavities for the Fermi laboratory’s International Linear Collider project. Single crystal Nb tubes may have superior performance compared to a polycrystalline tubes because the absence of grain boundaries may permit the use of higher accelerating voltages. In addition, Nb tubes that are subjected to the high temperature, high vacuum crystallization process are very pure and well annealed. Any impurity with a significantly higher vapor pressure than Nb should be decreased by the relatively long exposure at high temperature to the high vacuum environment. After application of the single crystal process, the surfaces of the Nb tubes are bright and shiny, and the tube resembles an electro polished Nb tube. For these reasons, there is interest in single crystal Nb tubes and in a process that will produce single crystal tubes. To convert a polycrystalline niobium tube into a single crystal, the tube is heated to within a few hundred C of the melting temperature of niobium, which is 2477 C. RF heating is used to rapidly heat the tube in a narrow zone and after reaching the operating temperature, the hotmore » zone is slowly passed along the length of the tube. For crystallization tests with Nb tubes, the traverse rate was in the range of 1-10 cm per hour. All the crystallization tests in this study were performed in a water-cooled, stainless steel chamber under a vacuum of 5 x10-6 torr or better. In earliest tests of the single crystal growth process, the Nb tubes had an OD of 1.9 cm and a wall thickness of 0.15 mm. With these relatively small Nb tubes, the single crystal process was always successful in producing single crystal tubes. In these early tests, the operating temperature was normally maintained at 2200 C, and the traverse rate was 5 cm per hour. In the next test series, the Nb tube size was increased to 3.8 cm OD and the wall thickness was increased 0.18 mm and eventually to 0.21 mm. Again, with these larger tubes, single crystal tubes were usually produced by the crystallization process. The power supply was generally operated at full output during these tests, and the traverse rate was 5 cm per hour. In a few tests, the traverse rate was increased to 10 cm per hour, and at the faster traverse rate, single crystal growth was not achieved. In these tests with a faster traverse rate, it was thought that the tube was not heated to a high enough temperature to achieve single crystal growth. In the next series of tests, the tube OD was unchanged at 3.8 cm and the wall thickness was increased to 0.30 mm. The increased wall thickness made it difficult to reach an operating temperature above 2,000 C, and although the single crystal process caused a large increase in the crystal grains, no single crystal tubes were produced. It was assumed that the operating temperature in these tests was not high enough to achieve single crystal growth. In FY 2012, a larger power supply was purchased and installed. With the new power supply, temperatures above the melting point of Nb were easily obtained regardless of the tube thickness. A series of crystallization tests was initiated to determine if indeed the operating temperature of the previous tests was too low to achieve single crystal growth. For these tests, the Nb tube OD remained at 3.8 cm and the wall thickness was 0.30 mm. The first test had an operating temperature of 2,000 C. and the operating temperature was increased by 50 C increments for each successive test. The final test was very near the Nb melting temperature, and indeed, the Nb tube eventually melted in the center of the tube. These tests showed that higher temperatures did yield larger grain sizes if the traverse rate was held constant at 5 cm per hour, but no single crystal tubes were produced even at the highest operating temperature. In addition, slowing the traverse rate to as low as 1 cm per hour did not yield a single crystal tube regardless of operating temperature. At this time, it appears that the wall thickness of the Nb tube rather than the operating temperature is the most important parameter to achieving single crystal growth. Single crystal growth was easily obtained with thinner wall tubes, but with thicker tubes, it was not achieved under varied growth conditions.« less
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