Synthesis with Zirconium Foil

The original two-step method described required zirconium sheet or foil in large excess to compensate for a surface-limited reaction. The sheet form also allows the ready separation of the product from unreacted metal. Although the litera- 

In the second stage, the ZrCl/ZrCl2 mixture, scraped from the foil in the dry box, is equilibrated isothermally with a 10-fold excess of fresh foil in a new reaction tube of the same type. The temperature is initially set at 600° and slowly raised to 800° over a period of 4-6 days, resulting in an essentially quantitative conversion to ZrCl, which can be recovered easily from the metal substrate in excellent purity. 

If only a small amount ( 1 g) of ZrCl or ZrBr is desired, it can be prepared directly in a single step with a 15-fold excess (by weight) of metal foil, the temperature being gradually raised from 400° to 800° over 10-14 days. 

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