1. Synthesize of Li-intercalated ZrNCl and ZrNBr Superconductor (Dikti Sandwich Program in IMR Tohoku Unv.) Andhy Setiawan Bandung Institute of Technology (ITB) 090121

2. Synthesize of Li-intercalated ZrNCl and ZrNBr Superconductor (Dikti Sandwich Program in IMR Tohoku Univ.) Sendai, January, 29th 2009 Have been presented on January, 21st 2009 by Andhy Setiawan In IWASA Lab. IMR Tohoku University Prof. Yoshihiro IWASA

3. Introduction  Dikti Sandwich Program is purposed to facilitate graduate students of Indonesia University to have a certain experience in overseas university  ITB IMR PECVD Lab. (ITB) IWASA Lab. (IMR) Getting new experiences  Synthesize of Li-intercalated ZrNCl and ZrNBr Superconductor

4. Synthesize Procedure and Its Apparatus Superconductor sample

5. Measurement and Its Apparatus Some Properties

6. Experiment Synthesize of ZrNCl : – ZrH2 (1g) + NH4Cl (10 g) Synthesize of ZrNCl (NMR) : –ZrH2 + NH4Cl ( 15 N) Synthesize of ZrNBr : –ZrH2 + NH4Br Purification of ZrNCl and ZrNBr Intercalation (synthesize of LixZrNCl, LixZrNBr) Measurement

7. Synthesize of ZrNCl Step 1 : Synthesize of ZrNCl 400 0 C600 0 C NH4Cl 10 g ZrH2 1 g N2N2

8. Purification of ZrNCl 750 0 C850 0 C ZrNCl + 0.1NH4Cl Pure ZrNCl Step 2 : Purification

9. Synthesize and Purification of ZrNCl (NMR) and ZrNBr 750 0 C850 0 C ZrH2 + 15 NH4Cl (ZrH2 + NH4Br) 750 0 C850 0 C ZrNCl + 0.1 15 NH4Cl (ZrNBr + 0.1 NH4Br) Pure ZrNCl (ZrNBr) Step 1 : Synthesize Step 2 : Purification ZrNBr

10. Intercalation Intercalation Li to ZrNCl Exp ZrNCl (mg) ZrNCl (mmol) BuLi (  L) Li (mmol)x 141.31.004000.40 Exp1145.41.034000.400.39 s-BuLi 140.51.005000.50 137.90.985000.500.51 140.31.001250.20 Exp2141.11.0062.50.10 n-BuLi 139.90.9936.250.0580.06 140.21.0012.50.02

11. Intercalation Intercalation Li to ZrNCl (NMR) Exp ZrNCl (mg) ZrNCl (mmol) BuLi (  L) Li (mmol)x Exp4246.81.7587.50.140.08 n-BuLi 313.42.23278.40.450.20 310.52.21276.10.440.20 Intercalation Li to ZrNBr (will be done) x = 0.05 – 0.15

12. Measurement Crystal Structure of ZrNCl (x-ray powder diffraction) Zr N Cl 60 0 b a c (003) (110) a = b = 3.602 Ǻ, c = 27.246 Ǻ 9.4749.2

13. Measurement Magnetization of LixZrNCl

14. Measurement Resistivity of LixZrNCl

15. Conclusion I have learned to Synthesize of Li-intercalated ZrNCl and ZrNBr superconductor. Measure the crystal structure, magnetization, and resistivity.

16. Acknowledgment Prof. Yoshihiro IWASA Miho EUMURA Yuichi KASAHARA and Superconductor Team in IWASA Lab. (Katsuki KOBAYASHI, Tsukasa KISHIUME, Takumi TAKANO) IWASA Lab. Member (T. TAKENOBU, H. SHIMOTANI, SATRIA ZB, H.T. YUAN, J. YE, S. INOUE, Y. YOMOGIDA, H. OKIMOTO, S. TSUDA, S. KIUCHI)

17. Thanks for Nice Moments