Final Report on Initial Samples Supplied by LLNL for Task 3.3 Binder Burnout and Sintering Schedule Optimisation
Sixteen of the twenty-one samples have been investigated using the scanning laser dilatometer. This includes all three types of samples with different preparation routes and organic content. Cracks were observed in all samples, even those only heated to 300 C. It was concluded that the cracking was occurring in the early part of the heat treatment before the samples reached 300 C. Increase in the rate of dilation of the samples occurred above 170 C which coincided with the decomposition of the binder/wax additives as determined by differential thermal analysis. A comparison was made with SYNROC C material (Powder Run 143), samples of which had been CIPed and green machined to a similar diameter and thickness as the 089mm SRTC pucks. These samples contained neither binder nor other organic processing aids and had been kept in the same desiccator as the SRTC samples. The CIPed Synroc C samples sintered to high density with zero cracks. As the cracks made up only a small contribution to the change in diameter of the sample compared to the sintering shrinkage, useful information could still be gained from the runs. The sintering curves showed that there was much greater shrinkage of the Type III samples containing only the 5% PEG binder compared to the Type I which contained polyolefin wax as processing aid. Slight changes in gradient of the sintering curve were observed, however, due to the masking effect of the cracking, full analysis of the sintering kinetics cannot be conducted. Even heating the samples to 300 C at 1.0 or 0.5 C/min could not prevent crack formation. This indicated that heating rate was not the critical parameter causing cracking of the samples. Sectioning of green bodies revealed the inhomogeneous nature of the binder/lubricant distribution in the samples. Increased homogeneity would reduce the amount of binder/lubricant required, which should in turn, reduce the degree of cracking observed during heating to the binder burnout temperature. A combination of: (1) use of a higher forming pressure, (2) reduction of organics content, (3) improvement in the distribution of the organic wax and binder components throughout the green body, could possibly alleviate cracking. Ultrasonic emulsification of the binder and wax with a small quantity of water prior to adding to the ball or attrition mill is advised to ensure more even distribution of the wax/binder system. This would also reduce the proportion of organic additives required. The binder burnout stage of the operation must first be optimized (i.e. production of pucks with no cracks) prior to optimization of the sintering stage.
- Research Organization:
- Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
- Sponsoring Organization:
- US Department of Energy (US)
- DOE Contract Number:
- W-7405-ENG-48
- OSTI ID:
- 15002964
- Report Number(s):
- UCRL-CR-139055-REV-1; TRN: US200420%%191
- Resource Relation:
- Other Information: PBD: 4 Jan 1999
- Country of Publication:
- United States
- Language:
- English
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